Report of an inter-laboratory comparison from the European Reference Laboratory for Food Contact Materials : ILC01-2014 : follow-up ILC01-2013 on proficiency testing on food simulant E containing a cocktail of potential migrant substances.
Date: 2015-11-11
Institutions: Institute for Health and Consumer Protection
Subjects: analytical chemistry, dangerous substance, food safety, packaging product, product safety, research body, research method, research report

Report of an Inter-laboratory 
Comparison from the European Union 
Reference Laboratory for Food Contact 
Materials 

ILC01-2014 – Follow-up ILC01-2013 
on Proficiency Testing on Food 
Simulant E containing a cocktail of 
potential migrant substances 

Juliana Silva Félix and Catherine Simoneau 

2 0 1 5  

Report EUR 27166 EN 

European Commission 
Joint Research Centre 
Institute for Health and Consumer Protection 

Contact information 
Catherine Simoneau 
Address: Joint Research Centre, Via Enrico Fermi 2749, TP 260, 21027 Ispra (VA) Italy 
E-mail: JRC-FCM@ec.europa.eu  

JRC Science Hub  
https://ec.europa.eu/jrc 

Legal Notice 
This publication is a Validated Methods, Reference Methods and Measurements Report by the Joint Research Centre,  
the European Commission’s in-house science service. It aims to provide evidence-based scientific support to the European 
policy-making process. The scientific output expressed does not imply a policy position of the European Commission. 
Neither the European Commission nor any person acting on behalf of the Commission is responsible for the use which 
might be made of this publication. 

All images © European Union 2015 

JRC95335 

EUR 27166 EN 

ISBN 978-92-79-47122-3 

ISSN 1831-9424 

doi:10.2788/455286 

Luxembourg: Publications Office of the European Union, 2015 

© European Union, 2015 

Reproduction is authorised provided the source is acknowledged. 

Abstract 

This report shows the results of the Interlaboratory Comparison ILC01-2014, a follow-up of the previous ILC01-2013. It is 
a Proficiency Testing (PT) on food simulant E spiked with potential migrant substances carried out by the European Union 
Reference Laboratory (EURL) for Food Contact Materials (FCM). Regulation (EU) No 10/2011 establishes food simulant E 
for  testing  migration  compliance  of  plastics  in  contact  with  dry  foodstuffs.  The  simulant  E  (Tenax®)  was  spiked  with  7 
substances  at  given  concentrations  tailored  for  this  exercise,  of  which  3  were  replaced  from  the  previous  year.  A  list 
containing  10  substances  in  which  7  were  effectively  present  in  the  simulant  was  distributed  to  the  participants. 
Homogeneity and stability studies were conducted. The main scope of this ILC01-2014 was to evaluate the improvement 
on the performance of the National Reference Laboratories (NRLs) for specific analysis of potential migrants in Tenax®. 
The participants should identify and quantify the substances spiked in the food simulant by using the analytical method of 
their choice. The z-score values, for each substance/laboratory, were obtained by the assigned value calculated with the 
results reported by the participants (robust mean). The participation of the laboratories in this follow-up on identification 
and quantification of the substances in food simulant E was very satisfactory regarding the number of received results as 
well as the significant improvement in the performance of the NRLs.  

 
EURL-FCM

    ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Table of content 

1. Summary ...................................................................................................................... 4

2. Introduction ................................................................................................................. 5

3. Scope............................................................................................................................ 6

4. Time frame ................................................................................................................... 7

5. Test material ................................................................................................................ 7

5.1. Sample preparation ................................................................................................ 7 

5.2. Homogeneity assessment ....................................................................................... 7 

5.3. Stability test ............................................................................................................ 8 

6. Instructions to the participants .................................................................................. 9

7. Evaluation of the results ............................................................................................. 9

7.1. General observations .............................................................................................. 9 

7.2. Statistical evaluation of results ................................................................................ 9 

7.2.1. Assigned value .................................................................................................... 9 

7.2.2. Target standard deviation .................................................................................... 9 

7.2.3. Kernel density .................................................................................................... 10 

7.2.4. z-score ............................................................................................................... 10 

8. Results ....................................................................................................................... 10

8.1. Preliminary considerations .................................................................................... 10 

8.2. Laboratories performance and z-scores ............................................................... 11 

9. Final conclusion ........................................................................................................ 22

Acknowledgements ....................................................................................................... 23 

10. References ............................................................................................................... 25

11. Annexes ................................................................................................................... 26

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

1. Summary 

Regulation (EU) No 10/2011 [1] established the food simulant E (Tenax®) for testing 
specific migration into dry foodstuffs. 

This report shows the results of the follow-up Interlaboratory Comparison Proficiency 
Testing  (PT)  ILC01-2014  on  the  food  simulant  E  containing  potential  migrant 
substances  carried  out  by  the  European  Union  Reference  Laboratory  (EURL)  for 
Food Contact Materials (FCM). 

In 2013 the EURL-FCM performed a first-time PT on identification and quantification 
of  unknown  substances  spiked  in  Tenax®.  The  participation  of  the  National 
Reference  Laboratories  (NRLs)  in  2013  was  satisfactory  (79%),  in  which  23 
participants  out  of  29 
the 
identification  of  the  unknown  substances,  48%  of  the  NRLs  (11  out  of  23)  could 
identify  correctly  all  the  7  substances.  In  relation  to  the  quantification,  32%  of  the 
NRLs (7 out of 22) could quantify all the substances within tolerance limits (z-scores 
≤ 2). Consequently, a follow-up for the ILC01-2013 was established with the NRLs. 

laboratories,  reported  results.  Regarding 

invited 

The  outcome  was  discussed and  a follow-up  was  established  in  consensus  with  all 
NRLs. The main scope of this ILC01-2014 was to evaluate the improvement on the 
performance of the NRLs for specific analysis of potential migrants in Tenax®. It was 
agreed that 3 substances from the previous exercise ILC01-2013 would be replaced. 
The  participants  had  to  identify  and  quantify  7  substances  spiked  in  the  food 
simulant,  and  using  the  analytical  method  of  their  choice,  including  general 
instructions provided by the EURL-FCM for the extraction of the substances spiked in 
Tenax® [2].  
The  test material was  prepared  by  the  EURL-FCM  and  consisted of  Tenax®  spiked 
with 7 potential migrant substances at one concentration level. For control purposes 
blank  Tenax®  from  the  same  batch  as  the  spiked  one  was  also  sent  to  the 
participants. A list containing the name of 10 chemical substances was distributed to 
the  participants, from which  7  would be  present  in the  food  simulant. The  choice  of 
the substances was based on relevant scientific literature [2-9]. 

The  substances  chosen  for  the  follow-up  ILC01-2014  were  benzophenone  (BP), 
caprolactam (CAP), dibutyl sebacate (DBS), bis(2-ethylhexyl)adipate (DEHA), bis(2-
ethylhexyl)  phthalate  (DEHP),  2,6-diisopropylnaphthalene  (DIPN)  and  2-ethyl-1-
hexanol  (ETHX).  The  concentration  of  each  substance  in  the  food  simulant  was 
tailored for the exercise. 
The homogeneity and stability studies for the substances in Tenax® were performed 
by the EURL-FCM. There were 36 participants from 28 countries to whom samples 
were dispatched. Twenty nine laboratories submitted results, of which 23 were NRLs, 
5 were Official Control Laboratories (OCLs) and one was the EURL-FCM itself. The 
participants  were  invited  to  report  four  replicate  measurements  under  repeatability 
conditions. 

The  assigned  values  were  obtained  as  consensus  values  after  applying  robust 
statistics  to  the  results  reported  by  the  participants.  Laboratory  results  were  rated 
with z-scores in accordance with ISO 13528 [10]. Reproducibility standard deviations 
(%)  calculated  by  DIN  38402  A45  [11]  for  the  different  substances  in  Tenax®  are 
summarised  below.  The  values  obtained  in  the  ILC01-2013  for  the  substances 
evaluated in this ILC01-2014 are also shown. 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

SML 
(mg/kg)   
[1] 

Assigned 
value (mg/kg) 
2013 

Reprod. SD % at 
the assigned 
value 2013 

Assigned 
value (mg/kg) 
2014 

Reprod. SD % at 
the assigned 
value 2014 

SUBSTANCES 

Benzophenone 

Bis(2-ethylhexyl) adipate 

Bis(2-ethylhexyl) phthalate 

0.6 

18 

1.5 

0.70 

8.37 

30.0 

32.5 

not performed 

not performed 

Caprolactam 

15 [T] 

11.89 

37.6 

Dibutyl sebacate 

60 [T] 

not performed 

not performed 

2,6-Diisopropylnaphthalene 

No SML* 

not performed 

not performed 

2-Ethyl-1-hexanol 

30 

9.24 

23.5 

* Substance not reported in the Positive List [1]. 

0.53 

4.09 

1.42 

9.59 

4.64 

1.42 

7.81 

36.4 

22.6 

30.7 

20.7 

23.2 

20.1 

29.6 

identification  and 
in 
The  participation  of 
quantification of BP, CAP,  DBS, DEHA, DEHP, DIPN and ETHX in food simulant E 
was  very  satisfactory  regarding  the  number  of  received  results  as  well  as  the 
significant improvement in the performance of the NRLs. 

follow-up  on 

laboratories 

this 

the 

2. Introduction 

Interlaboratory Comparisons (ILC) are widely used to evaluate the performance of an 
analytical  method,  as  well  as  the  ability  of  official  control  laboratories  to  deliver 
results with accuracy to their customers. ILC studies are also an essential element of 
laboratory  quality  assurance,  which  allows  individual  laboratories  to  compare  their 
analytical  results  with  those  from  other  laboratories  while  providing  them  objective 
standards to perform against. 

Regulation  (EC)  No  882/2004  of  the  European  Parliament  and  of  the  Council  [12] 
stipulated  the  organization  of  ILC  as  one  of  the  principal  responsibilities  of  the 
European Reference Laboratories (EURLs). 

In accordance with the above requirements the EURL-FCM organised in 2014 ILCs 
for the network of appointed NRLs. 

The scope of the ILCs for 2014 were discussed and established on plenaries with all 
NRLs. It was agreed that the objective of this ILC01-2014 would be a follow-up of the 
ILC01-2013 to evaluate the improvement of the  NRLs performance on identification 
and  quantification  of  7  potential  migrant  substances  in  food  simulant  E,  of  which 
would be given in a list containing 10 chemical substances (Annex 5). 

These  substances  were  chosen  because  they  were  reported  in  the  literature  as 
potential  migrants  from  food  packaging  materials  into  different  food  simulants, 
including  food  simulant  E  [2-9].  In  addition,  these  substances  were  suitable  for  this 
ILC01-2014  due  to  their  adequate  stability  in  that  particular  simulant.  Of  those,  7 
were  chosen  for  spiking  as  follows:  benzophenone  (BP),  a  light  stabilizer  (UV 
absorber),  caprolactam  (CAP)  is  the  monomer  of  polyamide-6,  dibutyl  sebacate 
(DBS),  a  plasticizer  recently  identified  as  migrant  coming  from  set-off  [13],  bis(2-
ethylhexyl)  adipate  (DEHA)  and  bis(2-ethylhexyl)  phthalate  (DEHP)  which  are  also 
used  as  plasticizers  in  plastic  food  packaging,  2,6-diisopropylnaphthalene  (DIPN) 
used  in  carbonless  copy  paper  and  2-ethyl-1-hexanol  (ETHX)  which  is  used  as 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

monomer  or  starting  substance.  Additional  characteristics  of  each  substance 
evaluated in the ILC01-2014 are shown in Table 1. 

Table 1. Substances used in the ILC01-2104. 

Substance 

CAS 

SML 
(mg/kg) [1] 

Exercise 

Molecular structure 

BP 

119-61-9 

0.6 

DEHA 

103-23-1 

18 

ILC01-2013 
ILC01-2014 

ILC01-2013 
ILC01-2014 

DEHP 

117-81-7 

1.5 

ILC01-2014 

CAP 

105-60-2 

15 (Total) 

ILC01-2013 
ILC01-2014 

DBS 

109-43-3 

60 (Total) 

ILC01-2014 

DIPN 

24157-81-1 

Not in 
Positive List 

ILC01-2014 

ETHX 

104-76-7 

30 

ILC01-2013 
ILC01-2014 

The participants were asked to identify and to quantify the potential migrants spiked 
in simulant E at one concentration level. The laboratories were free to use their own 
analytical  methods,  since  this  ILC  was  a  Proficiency  Testing.  They  were  invited  to 
report four replicate measurements in repeatability conditions. 

3. Scope 

This ILC was a follow-up from the previous exercise ILC01-2013. The scope of this 
ILC was a PT with the following objectives: 

 

to  evaluate  the  improvement  on  the  performance  of  the  NRLs  for  specific 
analysis of potential migrants in Tenax;  

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

 
 

to assess the NRLs performance on identification of the substances in Tenax; 
to control the NRLs performance on quantification of the substances in Tenax. 

The  assessment  of  the  measurement  results  was  undertaken  on  the  basis  of 
requirements laid down in international standards and guidelines [10, 14-16]. 

4. Time frame 

The ILC01-2014 was officially launched on the 8th of May 2014. Invitation letters and 
instructions (Annexes 1-8) were sent to the participants by mail. 

The  laboratories  were  invited  to  fill  in  a  letter  of  confirmation  of  their  participation 
(Annex 2). 

The  final  batch  of  Tenax®,  spiked  with  the  seven  substances  at  one  concentration 
level was prepared by the EURL-FCM in the beginning of May 2014. 

The homogeneity of the sample was checked and the sample kit was dispatched to 
the  participants  on  12th  of  May  2014,  together  with  the  shipping  kit  (Annex  3).  The 
participants were asked to fill in the confirmation of receipt of the sample (Annex 4). 

The deadline for reporting the results was set to 18th of July 2014. 

5. Test material 

The sample kit sent to the participants is shown in Table 2. The non-spiked (blank) 
Tenax®,  from  the  same  batch  as  the  spiked  one,  was  sent  to  the  participants  for 
control purposes. 

Table 2. Sample kit for the ILC01-2014 

Name 

TNX 

Blank TNX 

Sample 
Glass bottle containing Tenax® spiked with seven substances 
Glass vial containing non-spiked Tenax®, from the same batch of the spiked one 

5.1. Sample preparation 

Preparation and homogenization of the test materials were done by the EURL-FCM 
according to the procedure described in Annex 9. After spiking and homogenization, 
circa  20  g  portions  of the  spiked  Tenax®  were filled  into  glass  amber bottles;  which 
were placed in a thermostatic oven at 20°C. 

5.2. Homogeneity assessment 

The  sample  batch  (TNX)  was  tested  for  homogeneity  by  the  EURL-FCM.  Ten 
randomly selected test specimens for the sample TNX were analysed in duplicate to 
quantify BP, CAP, DBS, DEHA, DEHP, DIPN and ETHX. 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Homogeneity  was  evaluated  according  to  ISO  13528  [10]  and  IUPAC  International 
Harmonized Protocol [16] using the ProLab Software [17]. The homogeneity results 
and  their  statistical  evaluation  were  obtained  using  Horwitz  as  target  standard 
deviation (Annex 10). 

All test materials showed sufficient homogeneity. 

5.3. Stability test 

The  test  samples  were  monitored  for  stability  by  the  EURL-FCM  for  all  substances 
from the homogeneity assessment to the closing of the ILC01-2014. The stability was 
evaluated as  described  in  ISO  GUIDE 35:2006 [18].  Randomly  selected  specimens 
for sample TNX were stored at 3 different temperature conditions (4 °C, 20 °C and 40 
°C). 

The  evaluation  of  data  was  carried  out  by  performing  a  linear  regression  on  the 
experimentally  determined  concentrations  of  BP,  CAP,  DBS,  DEHA,  DEHP,  DIPN 
and ETHX (mean values) versus time (days). For a stable material, it is expected that 
the  intercept  is  (within  uncertainty)  equal  to  the  assigned  value,  whereas  the  slope 
does not differ significantly from zero. 

Using the linear regression equation: 

Y(BP, CAP, DBS, DEHA, DEHP, DIPN and ETHX mg/kg) = b0 +b1 X (time, days) 

the  slope  is  not  significantly  different  from  zero  if  the  following  requirement  is 
respected; 

where  

b1  
t0.95,n-2  

s(b1)    

is the slope obtained from the linear regression,  
is the Student’s t-factor for n-2 degrees of freedom and p = 0.95 (95% 
level of confidence) and  
is the uncertainty associated with the slope. 

This can be calculated as follows: 

The value of s (standard deviation of the time-points) can be obtained from: 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

where n is the number of points of the linear regression. 

The  stability  results  and  their  statistical  evaluation  are  given  in  Annex  11.  No 
significant trend was observed for the test sample at all temperature conditions (4 °C, 
20  °C  and  40  °C)  for  the  time  of  the  ILC01-2014.  It  was  concluded  that  the 
substances were stable for at least fifty days following their preparation. 

6. Instructions to the participants 

Instructions were given to all participants in the letters that accompanied the sample 
(Annex  5).  Laboratories  were  asked  to  report  4  quantitative  results  for  each 
substance using the unit of measure indicated in the electronic excel file (Annex  8). 
Participants were free to use their own analytical methods, or the general instructions 
sent  to  them  (Annex  6)  and  the  SOP  [2]  validated  in  the  previous  exercise  on 
Tenax®. 

7. Evaluation of the results 

7.1. General observations 

There were 36 participants to whom samples were dispatched (EURL-FCM, 30 NRLs 
+  5  OCLs  from  Germany  and  Spain).  The  results  were  submitted  by  23  NRLs,  5 
OCLs and 1 EURL-FCM. 

7.2. Statistical evaluation of results 

The  statistical  evaluation  of  the  results  was  performed  using  the  ProLab  software 
[16]. 

7.2.1. Assigned value 

A robust mean of the results reported by the participants was chosen as a consensus 
for  the  assigned  value  in  the  ILC01-2014.  The  assigned  value  was  evaluated 
according to Q-method/Hampel estimator (DIN 38402 A45) [11]. 

7.2.2. Target standard deviation 

The  value  of  target  standard  deviation  (σp)  determines  the  limits  of  satisfactory 
performance  in  an  ILC  test.  In  most  cases  Horwitz  SD  [10],  a  general  model 
commonly used for chemical application, is a good compromise but does not reflect 
different  levels  of  complexity  of  a  given  analytical  method.  If  the  target  standard 
deviation  is  not  chosen  realistically  the  interpretation  “satisfactory”,  “questionable” 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

and “unsatisfactory” would not be valid. On the other hand, the standard deviation of 
the reproducibility in collaborative trials can be considered as an appropriate indicator 
of the best agreement between laboratories. 

The σp of each substance evaluated in this ILC01-2014 was its reproducibility SD. 

7.2.3. Kernel density 

Kernel density  plots  were  additionally  used  to  identify  multi-modality  in  the  reported 
values' distributions.  Frequently  analytical results  from  a  collaborative  study  are  not 
normally distributed or contain values from different populations giving rise to multiple 
distribution modes. These modes can be visualised by using Kernel density plots [19, 
20].  Kernel  density  plots  were  computed  by  the  ProLab  software  [17]  from  the 
analytical results by representing the individual numeric values each as a normalized 
Gaussian distribution centered on the respective analytical value. The sum of these 
normal distributions formed then the Kernel density distribution. 

7.2.4. z-score 

Individual laboratory  performance  was  expressed  in terms  of  z-score  in  accordance 
with  ISO  13528  [10]  and  the  International  Harmonised  Protocol  [16].  The  z-scores 
compared the participant's deviation from the assigned value with the target standard 
deviation accepted for the PT: 

Where: 

xlab  
Xassigned  
σp  

is the measurement result (mean value) reported by a participant; 
is the assigned value; 
is the target standard deviation for proficiency assessment. 

The z-score can be interpreted as follow: 

|z|≤2    
2<|z|≤3  
|z|>3    

satisfactory result; 
questionable result; 
unsatisfactory result. 

In this exercise the z-scores calculated with the reproducibility SD as σp were used to 
assess the performance of the laboratories. 

8. Results 

8.1. Preliminary considerations 

The results were submitted by 29 laboratories, of which 23 were from NRL network, 5 
were OCLs (4 from Germany and 1 from Spain) and one was the EURL-FCM itself. 

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 passignedlabXxz)( 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

As  requested,  all  the  participants  reported  four  replicate  results  under  repeatability 
conditions. 

The participation of the laboratories was regarded as  satisfactory (81%) concerning 
the  number  of  received  results  (29  out  of  36).  Regarding  exclusively  the  NRLs,  the 
participation was 77% (23 out of 30). 

8.2. Laboratories performance and z-scores 

The  overall  performance  of  the  laboratories  regarding  the  identification  of  the 
substances  (qualitative  analysis)  is  shown  in  Table  3.  For  individual  substances, 
more  than  96%  of  the  qualitative  results  provided  were  correct.  In  this  follow-up 
exercise  the  laboratories  have  their  performance  improved  when  comparing  to  the 
identification reported in the ILC01-2013. 

Table 3. Qualitative analysis of the substances spiked in the food simulant E. 

ILC01-2013 

Total results 

Correct 

% Correct results 

ILC01-2014 

Total results 

Correct 

% Correct results 

BP 

30 

27 

90 

BP 

29 

28 

97 

CAP 

DEHA 

ETHX 

ACPH 

DTBP 

OCT 

30 

24 

80 

30 

30 

100 

30 

26 

87 

30 

22 

73 

30 

23 

77 

30 

25 

83 

CAP 

DEHA 

ETHX 

DBS 

DEHP 

DIPN 

28 

27 

96 

29 

28 

97 

29 

27 

96 

29 

28 

97 

29 

28 

97 

29 

28 

97 

Relating  to the  identification  of all  the 7  substances,  the  global performance  was  of 
76%, i.e. 22 laboratories out of 29 could identify correctly all the substances spiked in 
the  food  simulant.  Regarding  only  the  NRLs,  78%  (18  out  of  23  NRLs)  identified 
correctly all the substances, which represented an improvement of 30% compared to 
the previous ILC01-2013. 

Concerning  the  quantitative  analysis,  summaries  of  the  results  obtained  by  using 
ProLab  [17]  for  all  the  substances  with  their  robust  repeatability  SD  and  robust 
reproducibility  SD  calculated  according  to  Q-method/Hampel  estimator  (DIN  38402 
A45)  [11]  as  well  as  assigned  values,  target  standard  deviations  and  z-scores,  are 
given in Tables 4 and 5 and in Figures 1-7.  

Additionally,  the  results  sent  by  each  participant  for  each  of  the  evaluated 
substances, as well as the characteristics of the analytical method used, can be seen 
in the Annexes 12-18. 

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EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Table 4. Summary of results for the substances spiked in Tenax® calculated according to DIN 38402 A45. 

ProLab Results 

Assigned value = Robust Mean, mg/kg 

Robust Repeatability s.d., mg/kg 

Robust Reproducibility s.d., mg/kg 

Target SD (Reproducibility s.d.), mg/kg 

Target SD (Horwitz), mg/kg 

Rel. target SD (Reproducibility s.d.), % 

Rel. target SD (Horwitz), % 

Rel. Repeatability s.d., % 

Lower limit of tolerance, mg/kg 

Upper limit of tolerance, mg/kg 

Laboratories 

Test results 

BP 

0.533 

0.028 

0.194 

0.194 

0.094 

36.35 

17.58 

5.18 

0.146 

0.921 

28 

112 

CAP 

9.593 

0.448 

1.982 

1.982 

1.092 

20.66 

11.38 

4.67 

5.630 

13.556 

27 

108 

SUBSTANCES 

DEHA 

DEHP 

4.086 

0.187 

0.924 

0.924 

0.529 

22.63 

12.94 

4.57 

2.237 

5.935 

28 

112 

1.418 

0.104 

0.435 

0.435 

0.215 

30.67 

15.18 

7.33 

0.548 

2.288 

28 

112 

DBS 

4.641 

0.203 

1.075 

1.075 

0.589 

23.17 

12.70 

4.37 

2.490 

6.792 

28 

112 

DIPN 

1.418 

0.066 

0.287 

0.287 

0.215 

20.21 

15.18 

4.64 

0.845 

1.992 

28 

112 

ETHX 

7.811 

0.404 

2.311 

2.311 

0.917 

29.59 

11.74 

5.17 

3.189 

12.433 

27 

108 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Table 5. z-Scores obtained using the reproducibility SD as target SD. 

Laboratory 

ETHX 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0008 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

1.250 

-0.700 

-0.473 

-2.861 

1.883 

-* 

0.057 

0.858 

-0.005 

0.600 

0.748 

0.983 

0.718 

-0.223 

-0.978 

-0.513 

-0.399 

-0.453 

-0.009 

-0.143 

0.071 

1.325 

-1.556 

-* 

-0.464 

-2.706 

0.682 

-0.208 

0.276 

DIPN 

0.791 

-0.247 

0.416 

-0.456 

1.663 

-* 

-0.116 

-0.369 

0.721 

-0.229 

1.838 

8.893 

-0.142 

-0.299 

0.111 

0.416 

-0.081 

-0.779 

-0.421 

0.172 

-0.064 

3.380 

-3.221 

-2.310 

-0.674 

-3.988 

-0.003 

-0.822 

1.245 

BP 

0.757 

3.505 

0.435 

-1.259 

DEHP 

-0.237 

0.464 

0.062 

2.045 

-* 

17.078 

0.269 

-0.945 

0.805 

-0.042 

0.203 

0.499 

-0.455 

0.085 

-0.271 

-0.329 

0.028 

-0.639 

31.547 

19.510 

-0.068 

0.577 

-0.107 

-0.133 

0.525 

0.190 

0.074 

0.296 

1.067 

4.386 

-1.671 

-1.217 

-0.113 

-1.887 

-0.107 

-1.139 

1.325 

-0.565 

-0.024 

-0.329 

0.390 

0.269 

0.246 

-0.588 

1.172 

0.131 

1.781 

-2.028 

1.139 

-0.559 

-2.588 

-0.392 

0.401 

-* 

CAP 

0.016 

2.930 

-0.727 

-0.158 

0.161 

-* 

-0.446 

0.063 

-* 

0.282 

-0.439 

2.128 

-0.113 

-0.413 

-1.227 

-0.161 

-0.108 

-0.489 

-0.499 

0.987 

0.798 

0.667 

-2.935 

-0.727 

-0.516 

-4.232 

3.598 

0.707 

0.205 

DBS 

0.008 

0.094 

0.401 

-1.126 

1.703 

1.056 

2.278 

-0.478 

-1.038 

0.555 

-0.059 

-* 

-0.322 

0.522 

-0.224 

0.185 

1.029 

-0.319 

-0.510 

-0.089 

0.311 

1.096 

-1.813 

0.718 

-0.361 

-3.421 

-0.089 

-0.650 

-1.131 

DEHA 

-0.023 

-2.151 

0.659 

-0.574 

2.863 

-0.433 

-0.023 

-0.307 

-0.255 

0.483 

0.843 

4.988 

-0.428 

0.643 

-* 

0.288 

0.713 

-1.334 

-0.169 

0.305 

0.583 

1.866 

-2.230 

0.520 

-0.150 

-3.611 

-0.342 

-0.396 

0.286 

* Values not reported by the participants. 

Regarding  the  quantification  for  all  the  seven  substances  within  tolerance  limits 
(│z│≤ 2), 19 results out of 29 were satisfactory, which represented a success rate of 
66%. This percentage increases to 76% if the z-score values higher than 2 and lower 
or equal 3 are also taken into account. Concerning only the NRLs, 52% (12 out of 23) 
could quantify all the substances within tolerance limits. This value is 61% if also the 
laboratories  that  reported  results  for  5-6  substances  within  tolerance  limits  are 
included. If z-scores values 2<│z│≤3 are used for the calculation, so the % rises to 
74%. 

An overview about the number of z-score values within the tolerance limits (│z│≤ 2) 
and also z-scores between 2<│z│≤3, obtained in both PT on Tenax®, can be seen in 
Table 6. The delivery of results to a larger number of substances evaluated by each 

-13- 

 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

participant  was  higher  in  2014,  as  well  as  an  increase  in  the  number  of  z-scores 
within the limits of tolerance was observed. 

Table 6. Comparison of the number of z-scores obtained in both PTs on Tenax®. 

z-Score ILC01-2013 

Total results 

Number of scores, 2 < │z│ ≤ 3 

% 2 < │z│ ≤ 3 

Number of scores, │z│ ≤ 2 

% │z│ ≤ 2 

Total% 

z-Score ICL01-2014 

Total results 

Number of scores, 2 < │z│ ≤ 3 

% 2 < │z│ ≤ 3 

Number of scores, │z│ ≤ 2 

% │z│ ≤ 2 

Total % 

BP 

25 

2 

8 

20 

80 

88 

BP 

28 

0 

0 

25 

89 

89 

CAP 

DEHA 

ETHX 

ACPH 

DTBP 

OCT 

21 

3 

14 

18 

86 

100 

28 

1 

4 

23 

82 

86 

23 

0 

0 

19 

83 

83 

18 

0 

0 

17 

94 

94 

17 

1 

6 

15 

88 

94 

23 

1 

4 

20 

87 

91 

CAP 

DEHA 

ETHX 

DBS 

DEHP 

DIPN 

27 

3 

11 

22 

82 

93 

28 

3 

11 

23 

82 

93 

27 

2 

7 

25 

93 

100 

28 

1 

4 

26 

93 

97 

28 

3 

11 

23 

82 

93 

28 

1 

4 

23 

82 

86 

-14- 

 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure 1. Summary of the laboratories test results for BP with theirs repeatability SD 
(1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph). 

-15- 

    PROLab Plus Laboratory  LC0056LC0049LC0006LC0050LC0064LC0010LC0037LC0055LC0059LC0032LC0025LC0016LC0041LC0040LC0017LC0008LC0044LC0005LC0018LC0038LC0031LC0002LC0013LC0047LC0113LC0004LC0048LC0020mg/kg7.57.06.56.05.55.04.54.03.53.02.52.01.51.00.50.0Sample:Spiked TenaxMeasurand:benzophenoneMethod:DIN 38402 A45No. of laboratories:28Assigned value:0.533 mg/kg (Empirical value)Rel. target s.d.:36.35% (Empirical value)Rel. repeatability s.d.:5.18%Range of tolerance:0.146 - 0.921 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX BENZOPHE (TNX1)mg/kg876543210Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 0.533 ± 0.073 mg/kgMode 1: 0.312 mg/kg (19 %)Mode 2: 0.576 mg/kg (70 %)Mode 3: 1.232 mg/kg (4 %)Mode 4: 1.360 mg/kg (3 %)Mode 5: 6.120 mg/kg (1 %)Mode 6: 6.408 mg/kg (1 %)Mode 7: 6.800 mg/kg (1 %)Mode 8: 7.256 mg/kg (1 %)  PROLab Plus Laboratory  LC0056LC0049LC0006LC0050LC0064LC0010LC0037LC0055LC0059LC0032LC0025LC0016LC0041LC0040LC0017LC0008LC0044LC0005LC0018LC0038LC0031LC0002LC0013LC0047LC0113LC0004LC0048LC0020Z Score32302826242220181614121086420-2-4Measurand:benzophenoneLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure  2.  Summary  of  the  laboratories  test  results  for  CAP  with  theirs  repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph). 

-16- 

    PROLab Plus Laboratory  LC0056LC0049LC0032LC0005LC0050LC0055LC0041LC0040LC0010LC0018LC0031LC0037LC0006LC0025LC0038LC0002LC0013LC0007LC0113LC0017LC0048LC0064LC0047LC0044LC0020LC0004LC0059mg/kg22.020.018.016.014.012.010.08.06.04.02.00.0Sample:Spiked TenaxMeasurand:CaprolactamMethod:DIN 38402 A45No. of laboratories:27Assigned value:9.593 mg/kg (Empirical value)Rel. target s.d.:20.66% (Empirical value)Rel. repeatability s.d.:4.67%Range of tolerance:5.630 - 13.556 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX CAPROLAC (TNX1)mg/kg22.52017.51512.5107.552.50Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 9.593 ± 0.748 mg/kgMode 1: 1.215 mg/kg (3 %)Mode 2: 3.757 mg/kg (4 %)Mode 3: 9.157 mg/kg (89 %)Mode 4: 17.550 mg/kg (2 %)Mode 5: 20.700 mg/kg (2 %)  PROLab Plus Laboratory  LC0056LC0049LC0032LC0005LC0050LC0055LC0041LC0040LC0010LC0018LC0031LC0037LC0006LC0025LC0038LC0002LC0013LC0007LC0113LC0017LC0048LC0064LC0047LC0044LC0020LC0004LC0059Z Score43210-1-2-3-4-5Measurand:CaprolactamLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure  3.  Summary  of  the  laboratories  test  results  for  DBS  with  theirs  repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph) 

-17- 

    PROLab Plus Laboratory  LC0056LC0049LC0113LC0006LC0016LC0064LC0041LC0013LC0055LC0025LC0040LC0032LC0044LC0059LC0018LC0002LC0004LC0037LC0047LC0005LC0031LC0017LC0050LC0038LC0008LC0048LC0007LC0010mg/kg8.07.06.05.04.03.02.01.00.0Sample:Spiked TenaxMeasurand:Dibutyl sebacateMethod:DIN 38402 A45No. of laboratories:28Assigned value:4.641 mg/kg (Empirical value)Rel. target s.d.:23.17% (Empirical value)Rel. repeatability s.d.:4.37%Range of tolerance:2.490 - 6.792 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX DIBUTYLS (TNX1)mg/kg9876543210Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 4.641 ± 0.401 mg/kgMode 1: 0.963 mg/kg (4 %)Mode 2: 4.482 mg/kg (92 %)Mode 3: 7.254 mg/kg (5 %)  PROLab Plus Laboratory  LC0056LC0049LC0113LC0006LC0016LC0064LC0041LC0013LC0055LC0025LC0040LC0032LC0044LC0059LC0018LC0002LC0004LC0037LC0047LC0005LC0031LC0017LC0050LC0038LC0008LC0048LC0007LC0010Z Score3210-1-2-3-4Measurand:Dibutyl sebacateLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure 4. Summary of the laboratories test results for DEHA with theirs repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph) 

-18- 

    PROLab Plus Laboratory  LC0056LC0049LC0004LC0040LC0006LC0008LC0025LC0064LC0059LC0013LC0016LC0041LC0055LC0010LC0002LC0113LC0037LC0044LC0017LC0050LC0047LC0031LC0005LC0038LC0018LC0048LC0007LC0020mg/kg9.08.58.07.57.06.56.05.55.04.54.03.53.02.52.01.51.00.5Sample:Spiked TenaxMeasurand:diethylhexyladipateMethod:DIN 38402 A45No. of laboratories:28Assigned value:4.086 mg/kg (Empirical value)Rel. target s.d.:22.63% (Empirical value)Rel. repeatability s.d.:4.57%Range of tolerance:2.237 - 5.935 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX DIETHYLH (TNX1)mg/kg9876543210Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 4.086 ± 0.344 mg/kgMode 1: 0.756 mg/kg (3 %)Mode 2: 2.115 mg/kg (8 %)Mode 3: 3.987 mg/kg (86 %)Mode 4: 8.703 mg/kg (3 %)  PROLab Plus Laboratory  LC0056LC0049LC0004LC0040LC0006LC0008LC0025LC0064LC0059LC0013LC0016LC0041LC0055LC0010LC0002LC0113LC0037LC0044LC0017LC0050LC0047LC0031LC0005LC0038LC0018LC0048LC0007LC0020Z Score543210-1-2-3-4Measurand:diethylhexyladipateLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure 5. Summary of the laboratories test results for DEHP with theirs repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph) 

-19- 

    PROLab Plus Laboratory  LC0056LC0049LC0018LC0041LC0025LC0055LC0008LC0059LC0016LC0032LC0013LC0002LC0031LC0017LC0005LC0010LC0047LC0040LC0038LC0037LC0064LC0004LC0050LC0044LC0048LC0006LC0007LC0020mg/kg11.010.09.08.07.06.05.04.03.02.01.00.0Sample:Spiked TenaxMeasurand:Bis(2-ethylhexyl)phthalateMethod:DIN 38402 A45No. of laboratories:28Assigned value:1.418 mg/kg (Empirical value)Rel. target s.d.:30.67% (Empirical value)Rel. repeatability s.d.:7.33%Range of tolerance:0.548 - 2.288 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX BIS2-ETH (TNX1)mg/kg1211109876543210Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 1.418 ± 0.161 mg/kgMode 1: 0.504 mg/kg (6 %)Mode 2: 1.344 mg/kg (86 %)Mode 3: 8.868 mg/kg (5 %)Mode 4: 10.356 mg/kg (1 %)Mode 5: 11.016 mg/kg (1 %)  PROLab Plus Laboratory  LC0056LC0049LC0018LC0041LC0025LC0055LC0008LC0059LC0016LC0032LC0013LC0002LC0031LC0017LC0005LC0010LC0047LC0040LC0038LC0037LC0064LC0004LC0050LC0044LC0048LC0006LC0007LC0020Z Score2120191817161514131211109876543210-1-2-3-4Measurand:Bis(2-ethylhexyl)phthalateLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure  6.  Summary of the laboratories test results for  DIPN with theirs repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph) 

-20- 

    PROLab Plus Laboratory  LC0056LC0049LC0050LC0064LC0040LC0055LC0006LC0041LC0013LC0031LC0004LC0017LC0025LC0010LC0038LC0047LC0059LC0032LC0044LC0005LC0037LC0016LC0002LC0113LC0007LC0018LC0048LC0020mg/kg4.54.03.53.02.52.01.51.00.50.0Sample:Spiked TenaxMeasurand:2,6-DiisopropylnaphthaleneMethod:DIN 38402 A45No. of laboratories:28Assigned value:1.418 mg/kg (Empirical value)Rel. target s.d.:20.21% (Empirical value)Rel. repeatability s.d.:4.64%Range of tolerance:0.845 - 1.992 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX 26-DIISO (TNX1)mg/kg4.543.532.521.510.50Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 1.418 ± 0.106 mg/kgMode 1: 0.346 mg/kg (8 %)Mode 2: 1.350 mg/kg (85 %)Mode 3: 2.380 mg/kg (4 %)Mode 4: 3.280 mg/kg (1 %)Mode 5: 4.225 mg/kg (3 %)  PROLab Plus Laboratory  LC0056LC0049LC0050LC0064LC0040LC0055LC0006LC0041LC0013LC0031LC0004LC0017LC0025LC0010LC0038LC0047LC0059LC0032LC0044LC0005LC0037LC0016LC0002LC0113LC0007LC0018LC0048LC0020Z Score109876543210-1-2-3-4-5Measurand:2,6-DiisopropylnaphthaleneLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

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Figure  7.  Summary of the laboratories test results for ETHX with theirs repeatability 
SD (1st graph), Kernel density plot (2nd graph) and z-scores (3rd graph) 

-21- 

    PROLab Plus LaboratoryLC0006LC0056LC0049LC0032LC0004LC0037LC0005LC0055LC0040LC0038LC0031LC0064LC0044LC0041LC0016LC0010LC0047LC0113LC0017LC0059LC0025LC0018LC0013LC0020LC0002LC0048LC0007mg/kg14.013.012.011.010.09.08.07.06.05.04.03.02.01.0Sample:Spiked TenaxMeasurand:2-Ethyl 1-HexanolMethod:DIN 38402 A45No. of laboratories:27Assigned value:7.811 mg/kg (Empirical value)Rel. target s.d.:29.59% (Empirical value)Rel. repeatability s.d.:5.17%Range of tolerance:3.189 - 12.433 mg/kg (|Z Score| <= 2.00)Assigned valueMeanLimit of toleranceLimit of toleranceILC01-2014 TENAX 2-ETHYL1 (TNX1)mg/kg1614121086420-2Lower limit of toleranceUpper limit of toleranceAssigned value (Mean): 7.811 ± 0.879 mg/kgMode 1: 1.366 mg/kg (7 %)Mode 2: 7.396 mg/kg (93 %)  PROLab Plus Laboratory  LC0006LC0056LC0049LC0032LC0004LC0037LC0005LC0055LC0040LC0038LC0031LC0064LC0044LC0041LC0016LC0010LC0047LC0113LC0017LC0059LC0025LC0018LC0013LC0020LC0002LC0048LC0007Z Score3210-1-2-3Measurand:2-Ethyl 1-HexanolLimit of toleranceLimit of toleranceAssessment = DIN38402 A45; Assigned value = M; Target s.d. = S; |Z Score| <= 2 
 
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

9. Final conclusion 

The overall participation in the ILC01-2014 was satisfactory, with 29 laboratories (out 
of  36  invited  laboratories)  which  reported  results  (81%  of  participation).  Concerning 
NRLs, the participation was 77% (23 out of 30 laboratories). 

The  laboratories'  performance  concerning  the  qualitative  analysis  of  the  potential 
migrant substances in the simulant was satisfactory; with  more than 76% of correct 
identification  for  all  the  evaluated  substances.  Regarding  the  NRLs,  78%  of  the 
laboratories (18 out of 23 NRLs) identified correctly all the substances spiked in the 
Tenax®, which represented an improvement of 30% compared to the previous ILC01-
2013.  Taken  each  individual  substance  into  account,  more  than  96%  of  correct 
qualitative results were provided. 

Regarding  the  quantification  for  all  the  seven  substances  within  tolerance  limits 
(│z│≤ 2), 19 results out of 29 were satisfactory, which represented a success rate of 
66%. This percentage increases to 76% if the z-score values higher than 2 and lower 
or equal 3 are also taken into account. Concerning only the NRLs, 52% (12 out of 23) 
could quantify all the substances within tolerance limits. This value is 61% if also the 
laboratories  that  reported  results  for  5-6  substances  within  tolerance  limits  are 
included. If z-scores values 2<│z│≤ 3 are used for the calculation, so the % rises to 
74%. 

This exercise was the follow-up of the first Proficiency Testing carried out at EU level 
on food simulant E with the scope to evaluate the improvement of the performance of 
the National Reference Laboratories across the Member States. 

The  realization  of  this  follow-up  was  very  effective  since  most  laboratories  showed 
significant  improvement  in  the  identification  and  the  quantification  of  the  potential 
migrant  substances  in  food  simulant  E,  which  are  commonly  found  in  food  contact 
materials. 

-22- 

 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Acknowledgements 

The  NRLs  and  OCLs  participating  in  this  exercise  -  listed  below  -  are  kindly 
acknowledged. 

NRLs 

AUSTRIA 

BELGIUM 

BULGARIA 

CROATIA 

CYPRUS 

Austrian  Agency 
Lebensmittelsicherheit, Wien 

for  Health  and  Food  Safety 

(AGES), 

Institut 

für 

Institute of Public Health, ISSP-LP, Bruxelles 

National Centre for Public Health Protection, Sofia 

Croatian Institute of Public Health, Zagreb, Croatia 

Laboratory for Control of Food Contact Materials and Control of Toys 
Ministry of Health, State General Laboratory (SGL), Nicosia 

CZECH REPUBLIC 

NIPH  -  NRL  for  Food  Contact  Materials and  for  Articles  for children  under  3  years 
old, National Institute of Public Health (SZU’), Praha 

DENMARK 

Department of Food Chemistry, Danish Veterinary and Food Administration, Søborg 

ESTONIA 

FINLAND 

FRANCE 

GERMANY 

GREECE 

HUNGARY 

Health Protection Inspectorate - Central Laboratory of Chemistry, Tallinn 

Finnish Customs Laboratory, Espoo 

SCL Laboratoire de Bordeaux-Pessac, Pessac 

Bundesinstitut  für  Risikobewertung  (BFR)  (Federal  Institute  for  Risk  Assessment),                 
Berlin 

General  Chemical  State  Laboratory,  D’  Chemical  Service  of  Athens,  Section 
Laboratory of Articles and Materials in Contact with Foodstuffs, Athens 

Central  Agricultural  Office,  Food  and  Feed  Safety  Directorate,  Food  Toxicology 
National Reference Laboratory, Budapest 

IRELAND 

Public Analyst Laboratory - Sir Patrick Duns Hospital, Dublin 

ITALY 

Istituto  Superiore  di  Sanità,  Laboratorio  Esposizione  e  rischio  da  materiali,  c/o 
Dipartimento ambiente e connessa prevenzione primaria, Roma 

LUXEMBOURG 

Laboratoire  National  de  Santé,  Division  du  Controle  des  Denrées  Alimentaires, 
Luxembourg 

POLAND 

PORTUGAL 

SLOVAKIA 

SLOVENIA 

SPAIN 

Laboratory  of  Department  of  Food  and  Consumer  Articles  Research,  National 
Institute of Hygene, Warsaw 

ESB  Escola  Superior  de  Biotecnologia,  Universidade  Católica  Portuguesa, 
Packaging Department, Porto 

National  Reference  Centre  and  Laboratory  for  material  and  articles  intended  to 
come into contact with food, Regional Public Health Authority In Poprad (RUVZ) 

National  Institute  of  Public  Health  of  Republic  of  Slovenia,  Department  of  Sanitary 
Chemistry, Ljubijana 

Centro  Nacional  de  Alimentación,    Agencia  Española  de  Seguridad  Alimentaria  y 
Nutrición (AESAN), Madrid 

THE NETHERLANDS 

Food and Consumer Product Safety Authority (VWA), Ministry of Economic Affairs, 
Agriculture and Innovation, Groningen 

UNITED KINGDOM 

The Food and Environment Research Agency, York 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

OCLs 

GERMANY 

Landesamt für Verbraucherschutz Sachsen-Anhalt, Halle 

GERMANY 

Landesuntersuchungsanstalt für das Gesundheits- und Veterinärwesen Sachsen, Dresden 

GERMANY 

Chemisches und Veterinäruntersuchungsamt, Fellbach 

GERMANY 

Bayerisches Landesamt für Gesundheit und Lebensmittelsicherheit, Erlangen 

SPAIN 

Laboratorio de Salud Pública, Alicante 

-24- 

 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

10. References 

[1] 

[2] 

[3] 

[4] 

[5] 

[6] 

[7] 

[8] 

[9] 

Regulation  EC10/2011  of  the  European  Parliament  and  the  Council  of  14  January  2011  on  plastic 
materials and articles intended to come into contact with food 

Beldì et al. 2012. Development of a harmonised method for specific migration into the new simulant for 
dry  foods  established  in  Regulation  10/2011;  Establishment  of  precision  criteria  from  an  EU 
interlaboratory comparison organised by the EURL Food Contact Materials for the quantification from 
and migration into poly(2,6-diphenyl phenylene oxide). European Commission - Joint Research Centre 
- Institute for Health and Consumer Protection - EUR 25680. doi:10.2788/76804 

Félix et al. 2013. Report of an Interlaboratory Comparison from the European Reference Laboratory for 
Food Contact Materials: ILC001-2013 – Proficiency Testing on Food Simulant E containing a cocktail of 
potential migrant substances. European Commission - Joint Research Centre - Institute for Health and 
Consumer Protection - EUR 26468 EN. doi:10.2788/6263 

Félix et al. 2012. Analytical Bioanalytical Chemistry 403:2869-2882. DOI: 10.1007/s00216-012-5965-z 

Canellas et al. 2012. Journal of Chromatography A 1235: 141-148. DOI: 10.1016/j.chroma.2012.02.039 

Poças et al. 2011. Food Control 22: 303-312. DOI:10.2788/76804 

Suciu et al. 2013. Food Chemistry 141: 4146-4151. DOI:  10.1016/j.foodchem.2013.07.014 

Triantafyllou et al. 2002. Analytica Chimica Acta 467: 253-260. DOI: 10.1016/S0003-2670(02)00189-7 

Bradley et al. 2010 Food Additives and Contaminants 27: 262-271. DOI: 10.1080/02652030903232746 

[10] 

ISO 13528:2005; Statistical Methods for Use in Proficiency Testing by Interlaboratory Comparisons 

[11] 

DIN 38402 A45 Ringversuche zur externen Qualitätskontrolle von Laboratorien. 

[12] 

Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 on official 
controls performed to ensure the verification of compliance with feed and food law, animal  health and 
animal welfare rules 

[13] 

Aznar et al. 2015. Dyes and Pigments 114: 85-92. DOI: 10.1016/j.dyepig.2014.10.019 

[14] 

M. Thompson, Analyst, (2000), 125, 385-386 

[15] 

T. Linsinger et al., Accreditation and Quality Assurance in Analytical Chemistry (2001), 6, 20-25 

[16] 

The International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories 
by M. Thompson et al., Pure and Applied Chemistry (2006), 78, 145–196 

[17] 

ProLab Software – QuoData, Drezden – www.quodata.de 

[18] 

ISO GUIDE 35:2006; Reference materials–General and statistical principles for certification. 

[19] 

[20] 

AMC,  Representing  data  distributions  with  kernel  density  estimates.  AMC  Technical  Brief,  2006, 
http://www.rsc.org/images/brief4_tcm18-25925.pdf 

P.J. Lowthian and M. Thompson, Bump-Hunting for the proficiency tester - searching for multimodality. 
The Analyst, 2002. 127: p. 1359,  

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

11. Annexes 

Annex 1. 

Invitation letter to the laboratories to ILC01-2014 

Annex 2.  

Letter for confirmation of participation to ILC01-2014 

Annex 3. 

Shipping kit letter accompanying the sample TNX1 to ILC01-2014 

Annex 4.  

Letter of confirmation of receipt of the sample to ILC01-2014 

Annex 5.  

Letter Instructions for the compilation of the results from ILC01-2014 

Annex 6.   General instructions for ILC01-2014 

Annex 7.   Method information used for the participant during the ILC01-2014 

Annex 8. 

Form for the compilation of the results in non-electronic format 

Annex 9. 

Procedure for the preparation of the spiked food simulant E 

Annex 10.  Results of the homogeneity study 

Annex 11.  Results of the stability study and the statistical evaluation 

Annex 12.  Benzophenone values reported by the participants 

Annex 13.  Bis(2-ethylhexyl) adipate values reported by the participants 

Annex 14.  Bis(2-ethylhexyl) phthalate values reported by the participants 

Annex 15.  Caprolactam values reported by the participants 

Annex 16.  Dibutyl sebacate values reported by the participants 

Annex 17. 

2,6-Diisopropylnaphthalene values reported by the participants 

Annex 18. 

2-Ethyl-1-hexanol values reported by the participants 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant 
substances 

Annex 1. Invitation letter to the laboratories to ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Ispra, 07th May 2014 

Dear Madam, Sir 

Interlaboratory Comparison (ILC) exercise on food simulant E – ILC01-2014 
Follow-up ILC001-2013 

On behalf of the EURL for food contact materials, I would like to invite you to participate in the  follow-up of ILC 
exercise for the determination of substances in food simulant E which is due to start by the middle of May. As 
agreed in the last EURL-NRL FCM plenary, the scope of this ILC exercise is a Proficiency Testing, laboratories 
are free to use their own methods. 

This ILC aims at the extraction and identification/quantification of substances from food simulant E. There is no 
migration experiment in this exercise. 

You will receive a list of ten substances. Seven substances from that list have been spiked into the food simulant 
E.  You  need  to  identify  and  quantify  them.  Regarding  the  quantification,  we  tried  to  maintain  similar  GC-MS 
response  among  all  the  substances  (similar  peak  heights). So,  consequently  the  exercise  may  not  necessarily 
target only around SMLs. The concentration of the substances will range up to 10-15 mg/kg. 

I  would  like to  remind  you  that  it  is  a duty  for  you  as  an  NRL-FCM  to  participate  in  the  ILCs  organised  by  the 
EURL-FCM since the work programme is decided with your agreement. For  this reason we require all of you to 
actively participate in this exercise. There is no charge for participation.  

We have pre-registered everyone, which means we will send test kits to all of you. We however need to receive 
the proformat  of  your  participation for our own administrative purposes. Kindly send back it  by  26th  May  to: 
Juliana Silva Félix (juliana.silva-felix@ec.europa.eu). 

The samples will be sent to you in the middle of May. You will find additional information on the form “Shipping kit 
ILC01-2014” that you will receive by e-mail. You will also receive more detailed instructions for the compilation of 
the  results  on  the  form  "Instructions  Excel  ILC01-2014".  The  deadline  for  submission  of  results  is  18th  July 
2014. 

If you have any question, please contact Juliana Silva Félix (juliana.silva-felix@ec.europa.eu). 

Sincerely yours, 

Catherine Simoneau 
Operating Manager, European Reference Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit Chemical Assessment and Testing, T.P. 260 
Ispra VA 21020 Italy 

Cc:  

P. Aguar (JRC), D. Rembges (JRC) 
B. Schupp (SANCO) 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 2. Letter for confirmation of participation to ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Ispra, 07th May 2014 

Participation to EURL-FCM ILC01-2014 
Interlaboratory comparison exercise on food simulant E 
Follow-up ILC001-2013 

CONFIRMATION OF PARTICIPATION 

Your Name: 

Organization: 

Address:  

E-mail:  

Phone:  

Kindly send back this proformat to: Juliana Silva Félix (juliana.silva-felix@ec.europa.eu) by  the  26th 
May 2014. 
The  samples  will  be  sent  to  you  in  the  middle  of  May.  You  will  find  additional  information  in  the  kit 
sent. The deadline for submission of results is 18th July 2014. 

Sincerely yours, 

Catherine Simoneau 
Operating Manager, European Reference Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit Chemical Assessment and Testing, T.P. 260 
Ispra VA 21020 Italy 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 3. Shipping kit letter accompanying the sample TNX1 to ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Ispra, 07th May 2014 

Shipping kit ILC01-2014  
exercise on food simulant E - EURL-FCM ILC01-2014 
Follow-up ILC001-2013 

Shipping kit - samples 

  Sample  TNX  –  One  glass  bottle  containing  food  simulant  E  spiked  with  the  unknown 

substances 

  Blank TNX – For control purposes: one glass vial containing the food simulant E not spiked, 

from the same batch of the spiked one 

Shipping kit – documentation (send by email) 

  Letter of confirmation of receipt of the sample; 

  General instructions to perform the calibration and the extraction 

  Letter with instructions for compilation of the results; 

  Electronic excel file” ILC01-2014 test results TNX.xls”. 

Storage 

  Sample TNX – could be stored between 4 and 20°C. 

Instructions 

Use the Excel form “ILC01-2014 test results TNX.xls” to provide your results in 4 replicates. 

Sincerely yours, 

Catherine Simoneau 
Operating Manager, EU Reference Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit Chemical Assessment and Testing, T.P. 260 
Ispra VA 21020 Italy 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 4. Letter of confirmation of receipt of the sample to ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Ispra, 7th May 2014 

Participation to ILC01-2014 on food simulant E 
Follow-up ILC001-2013 

CONFIRMATION OF RECEIPT OF THE SAMPLE 

Please return this form to confirm that the sample package has arrived. In case the package is 
damaged, please state this on the form and contact us immediately. 

Your Name: 

Organization: 

E-mail: 

Phone: 

Any remarks 

..…..……………………. 

Date arrival package 

..…..……………………. 

Signature 

..…..……………………. 

Kindly send back this form to: Juliana Silva Félix (juliana.silva-felix@ec.europa.eu) 

Sincerely yours, 

Catherine Simoneau 
Operating Manager, ЕU Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit CAT, T.P. 260 
Ispra VA 21020 Italy 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 5. Letter Instructions for the compilation of the results from ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Ispra, 7th May 2014 

Instructions Excel ILC01-2014 

Instructions for compilation of the results for ILC01-2014 on food simulant E 
Follow-up ILC001-2013 

DEADLINE: Wednesday, July 18th 2014 

You can find in the table below a list of ten substances. Seven substances from that list are spiked in 

the food simulant E. You need to identify and quantify them. 

SUBSTANCES 

1-Octene 

Bis(2-ethylhexyl) adipate 

Dibutyl sebacate 

Benzophenone 

Bis(2-ethylhexyl) phthalate 

Erucamide 

2-Ethyl-1-hexanol 

2,6-Diisopropylnaphthalene 

Methyl stearate 

Caprolactam 

CAS number 

111-66-0 

103-23-1 

109-43-3 

119-61-9 

117-81-7 

112-84-5 

104-76-7 

24157-81-1 

112-61-8 

105-60-2 

Perform four replicates for the sample TNX and fill your four results in the Excel file (ILC01-2014 test 

results TNX.xls). The laboratory code is reported in the sample bottle. Send the results back by e-mail 
to Juliana S. Félix (juliana.silva-felix@ec.europa.eu) by July 18th 2014. 

Sincerely yours, 

Catherine Simoneau 
Operating Manager, EU Reference Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit Chemical Assessment and Testing, T.P. 260 
Ispra VA 21020 Italy 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 6. General instructions for ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

GENERAL INSTRUCTIONS FOR ILC01-2014 

Determination of Substances in Food Simulant E 

1 

Introduction 

These  general  instructions  describe  the  methods  for  the  extraction  procedure  with  subsequent 
quantification of the substances from the Tenax®. 

It  is  important  to  highlight  that  this  Interlaboratory  Comparison  (ILC01-2014)  is  a  follow-up  of  the 

ILC001-2013. 

As  this  exercise  is  a  Proficiency  Test,  the  participants  are  free  to  use  the  analytical  method  of  their 

choice. 

Calibration 

2 
Calibration  is  done  by  spiking  Tenax®  with  appropriate  amounts  of  a  multianalyte  standard  solution. 

After 1h the substances are extracted using the extraction procedure described in the Section 3. 
Pay  attention:  Use  your  own  Tenax®  to  do  the  calibration.  The  BLANK  TNX  should  be  used  as 

control in order to have a background of the sample TNX. 

2.1 

Solutions 

2.1.1  Stock solutions 

Prepare  stock  solutions  with  each  analytical  standard  and  appropriate  solvent.  Calculate  the  exact 

concentration of the substances in µg/mL. 

2.1.2  Multianalyte standard solution in acetone 
This  solution  is  used  to  spike  your  own  Tenax®  and  carry  out  the  calibration.  Pipette  appropriate 

amounts of each stock solution into a  volumetric flask and fill the flask up to the mark with  acetone. 

Calculate the exact concentration of the substances in µg/mL. 

2.1.3  Acetone extraction solution containing the internal standard 

Pipette an appropriate amount of the internal standard stock solution into a volumetric flask and fill the 

flask up to the mark with acetone. Calculate the exact concentration of the internal standard in µg/mL. 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Preparation of the calibration curve 

2.2 
  Weight 1.0 g of clean Tenax® in 40 mL vials; 
  Spike the Tenax® with appropriate amounts of the multianalyte standard solution using the digital 

pipette or syringe; 

  Extract the substances from Tenax® as reported in Section 3; 
  Use the Tenax® without spiking as blank and extract it as in Section 3. 

Extraction of the substances from the spiked Tenax® 

3 
The substances are extracted twice from the Tenax® with an extraction solution containing an internal 

standard.  The  extractions  carried  out  with  the  acetone  extraction  solution  provided  recoveries  in  the 

range of 80-120%for all the spiked substances. 

Procedure steps: 
  Transfer 1.0 g of the spiked Tenax® into a 40 mL glass vial; 

  Add 20 mL of the acetone extract solution (containing the internal standard); 

  2  min  in  ultrasonic  bath  (20  ºC,  40kHz,  100%  power)  (or  alternatively,  manually  shaking  for  1-2 

min); 

  Leave it for 5 min without shaking; 
  Gently  decant  the  first  acetone  extract  from  the  Tenax®  into  a  new  40  mL  glass  vial  (it  is  also 

possible decant the extract through a Büchner funnel with a glass microfiber filter); 

  Repeat this extraction procedure using once again 20 mL of the acetone extract solution; 

  Collect the second extract in the same 40 mL glass vial; 

  Evaporate the acetone extract (approx.. 40 mL) under the nitrogen stream to around 5 mL; 

  Filter the extract using a PTFE filter (0.2 µm) into a 2 mL glass vial; 

 

Inject  the  concentrated  extract  into  a  gas  chromatography-mass  spectrometry  (GC-MS). 

Quantification is done using an internal standard and in SIM mode. 

4. Quantification 

4.1 

Analysis of calibration standard solutions 

Inject the extracts from calibration (2.2) into a GC-MS. Integrate peaks and measure peak area for the 

substances  of  interest  and  also  for  the  internal  standard.  Construct  a  calibration  function  by  plotting 

the analytes concentration against the ratio of the peak area of the analytes and the peak area internal 

standard in the calibration solutions. Calculate the regression parameters and correlation coefficient.  

The calibration curve shall be linear and the correlation coefficient shall be 0,99 or better.  If either of 

the two requirements is not met, fresh standard solutions shall be prepared from the original standard 

solutions. Analysis of the solutions and construction of the calibration graph have to be repeated. 

4.2  

Analysis of samples  

Inject the sample solutions, prepared in Section 3, under the same chromatographic conditions used 

for  the  calibration  solutions.  Measure  the  area  of  the  peaks  for  calculation  of  the  substance 

concentrations against established in 4.1 regression. Internal standard is used to compensate for the 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

losses of analytes caused by sample handling, adsorption effects etc. 

Evaluation of data 

4.3  
Calculate of the substance concentration in the spiked Tenax® sample in mg/kg: 

Concentration in Tenax® [mg/kg] = 

Where: 

C  

W  

is the substance mass in µg derived from the calibration curve, and 

is the weight of sample taken in g. 

5  

Confirmation 

For confirmation of peak identity the retention time and a ratio between target and qualifier ions shall 

be taken into account. 

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WC  
 
 
 
 
 
 
EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 7. Method information used for the participant during the ILC01-2014 

EUROPEAN COMMISSION 
GENERAL DIRECTORATE JRC 
JOINT RESEARCH CENTRE 
Institute for Health and Consumer Protection – IHCP 
Chemical Assessment and Testing Unit 

Dear Madame/Sir 

ILC01-2014 

In  order  to  have  a  better  understanding  about  the  different  analytical  methods  used  to  extract  the  studied 
substances from Tenax®, EURL-FCM need to gather information about the analytical method used. 

Therefore  we  kindly  ask  you  to  fill  the  following  table  and  to  send  it  by  e-mail  together  with  your  results  to: 
juliana.silva-felix@ec.europa.eu 

Cleaning 
Food Simulant E cleaning procedure applied: 

Sample preparation 
Solvents used for extraction: 

Extraction procedure: 

Internal standard: 

Calibration 
By spiking food simulant E or standard solution in solvents: 

Analytical technique used 
Gas chromatography 
Analytical Column: 

Oven temperature programme: 

Detector used: 

SIM or SCAN: 

Other analytical techniques used: 

Thank you for your collaboration. 

Sincerely yours, 

Liquid chromatography 
Mobile phase: 

Gradient: 

Column: 

Detector: 

Catherine Simoneau 
Operating Manager, European Reference Laboratory for Food Contact Materials 
European Commission, DG-Joint Research Centre 
Institute for Health and Consumer Protection 
Unit Chemical Assessment and Testing, T.P. 260 
Ispra VA 21020 Italy 

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EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 8. Form for the compilation of the results in non-electronic format 

FCM EURL-NRL ILC01-2014 on Food Simulant E  

TEST RESULTS 

Lab Code - LC00........ 

   Identification and quantification of the substances in the spiked food simulant E 

   No. 

Substance name 

CAS 

Replicate 1 

Replicate 2 

Replicate 3 

Replicate 4 

remark 

Concentration in the sample TNX (mg/kg) 

1 

2 

3 

4 

5 

6 

7 

Place and date 

.................................. 
Laboratory Manager 

............................... 
Signature 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 9. Procedure for the preparation of the spiked food simulant E 

1. Washing of the 10 L round bottom flask:  

  10 L mixing round bottom flask was washed in a dish washer,  then filled with 

the deionised water (resistivity 18 MΩ.cm @ 25 °C) and mixed; 

  The water was removed; 
  The  mixing  bottle  was  filled  with  0.5  L  of  pentane  (Aldrich,  HPLC  grade  + 

99%) and shaked; 
  Pentane was removed. 

2. Preparation of the spiking solutions: 

a) Stock  solution  of BP,  DBS,  DEHA,  DEHP,  DIPN  and  ETHX  prepared  in  acetone 
(approx. 1000 mg/L)  

  50  mg  of  each  compound  was  weighted  separately  into  a  50  mL  class  A 

volumetric flask and dissolved in acetone; 
the flask was filled up to the mark with acetone. 

 

b) Stock solution of CAP in ethanol (approx. 1000 mg/L) 

  50  mg  of  CAP  was  weighted  into  a  50  mL  class  A  volumetric  flask  and 

dissolved in ethanol; 
the flask was filled up to the mark with ethanol. 

 

c) Spiking solution of BP, CAP, DBS, DEHA, DEHP, DIPN and ETHX in pentane 

  0.6 mL of BP, 10 mL of CAP, 5 mL of DBS, 4.5 mL of DEHA, 1.5 mL of DEHP, 
1.4  mL  of  DIPN  and  8  mL  of  ETHX  (from  the  stock  solutions)  were  pipetting 
into the 2 L volumetric flask; 
the flask was filled up to the mark with pentane. 

 

3. Preparation of the spiking food simulant E: 

  1 kg of the cleaned simulant was weighted and transferred into the 10 L round 

bottom flask; 

  2 L of the spiking solution in pentane was add to the simulant; 
  The  volumetric  flask  was  rinsed  by  other  2  L  of  pentane  and  all  the  solvent 

was collected into the round bottom flask; 

  The flask was closed and the simulant was mixed continuously for 2.5 hours; 
  The  flask  was  opened  and  the  simulant  was  mixed  till  the  complete 

evaporation of the pentane (approximately 3 days). 

  An amount of ca. 20 g were distributed into amber bottles, which were placed 

into a thermostatic oven at 20 °C. 

  Ten  randomly  selected  test  specimens  for  the  sample  TNX  were  tested  for 

homogeneity before being sent to participants. 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 10. Results of the homogeneity study. 

Analyte 

Mean 
(mg/kg) 

Mode 
s(target) 

s(samples) 
[%] 

s(target) 
[%] 

ISO 13528 
Check for sufficient 
homogeneity 

Harmonized Protocol 
Test on significant 
heterogeneity 

BP 

CAP 

DBS 

DEHA 

DEHP 

DIPN 

ETHX 

0.627 

Horwitz 

0.000 

17.161 

9.616 

Horwitz 

0.953 

11.379 

5.013 

Horwitz 

2.154 

12.551 

4.287 

Horwitz 

0.919 

12.850 

1.423 

Horwitz 

1.533 

15.169 

1.424 

Horwitz 

0.132 

15.169 

7.445 

Horwitz 

1.986 

11.826 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

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EURL-FCM                           ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 11. Results of the stability study and the statistical evaluation. 

Substance 

Temperature 

Intercept 

Slope 

s(b1) 

t(α=0.95,n-2)·s(b1) 

|b1|< t(α=0.95,n-2)·s(b1) 

Up to 50 days 

BP 

CAP 

DEHA 

ETHX 

DBS 

DEHP 

DIPN 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

4 ºC 

20 ºC 

40 ºC 

0.6252 

0.0003 

0.0003 

0.6322 

-0.0005 

0.0002 

0.6372 

-0.0006 

0.0003 

9.5574 

-0.0049 

0.0015 

9.6787 

-0.0135 

0.0034 

9.6716 

-0.0189 

0.0078 

3.6252 

-0.0080 

0.0055 

3.6483 

-0.0085 

0.0048 

3.6038 

-0.0060 

0.0056 

5.2199 

-0.0093 

0.0102 

4.9503 

-0.0030 

0.0191 

5.1936 

-0.0282 

0.0223 

5.1499 

-0.0121 

0.0061 

5.1963 

-0.0123 

0.0065 

5.1552 

-0.0093 

0.0064 

1.7243 

-0.0053 

0.0020 

1.7183 

-0.0049 

0.0035 

1.6914 

-0.0036 

0.0024 

1.6626 

-0.0025 

0.0017 

1.6594 

-0.0029 

0.0018 

1.6416 

-0.0029 

0.0019 

0.0012 

0.0007 

0.0014 

0.0063 

0.0145 

0.0334 

0.0176 

0.0152 

0.0179 

0.0324 

0.0609 

0.0709 

0.0195 

0.0208 

0.0203 

0.0063 

0.0151 

0.0076 

0.0055 

0.0058 

0.0061 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

OK 

-39- 

 
 
 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 12. Benzophenone values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0008 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

0.730 

1.200 

0.600 

0.292 

0.566 

0.350 

0.662 

0.500 

0.580 

0.660 

7.260 

0.530 

0.620 

0.450 

0.590 

0.627 

0.580 

0.530 

0.640 

0.680 

1.390 

0.222 

0.334 

0.510 

0.160 

0.570 

0.320 

0.850 

0.760 

1.220 

0.630 

0.293 

0.571 

0.350 

0.708 

0.500 

0.560 

0.620 

6.800 

0.520 

0.620 

0.550 

0.480 

0.634 

0.570 

0.570 

0.591 

0.800 

1.386 

0.202 

0.265 

0.532 

0.170 

0.460 

0.300 

0.810 

0.700 

1.200 

0.610 

0.285 

0.592 

0.350 

0.730 

0.500 

0.560 

0.640 

6.120 

0.520 

0.660 

0.550 

0.430 

0.619 

0.560 

0.560 

0.565 

0.720 

1.356 

0.216 

0.276 

0.529 

0.170 

0.500 

0.310 

0.480 

0.530 

1.230 

0.630 

0.287 

0.612 

0.350 

0.657 

0.600 

0.590 

0.600 

6.410 

0.510 

0.680 

0.500 

0.530 

0.660 

0.570 

0.530 

0.566 

0.760 

1.401 

0.197 

0.314 

0.474 

0.170 

0.520 

0.320 

1.020 

0.680 

1.213 

0.618 

0.289 

0.585 

0.350 

0.689 

0.525 

0.573 

0.630 

6.648 

0.520 

0.645 

0.513 

0.508 

0.635 

0.570 

0.548 

0.591 

0.740 

1.383 

0.209 

0.297 

0.511 

0.168 

0.513 

0.313 

0.790 

0.103 

0.015 

0.015 

0.004 

0.021 

0.000 

0.036 

0.050 

0.015 

0.026 

0.494 

0.008 

0.030 

0.048 

0.068 

0.018 

0.008 

0.021 

0.035 

0.052 

0.019 

0.012 

0.032 

0.027 

0.005 

0.046 

0.010 

0.226 

15.1 

1.2 

2.4 

1.3 

3.6 

0.0 

5.1 

9.5 

2.6 

4.1 

7.4 

1.6 

4.7 

9.3 

13.5 

2.8 

1.4 

3.8 

5.9 

7.0 

1.4 

5.6 

Acetone 

Hexane 

Acetone 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

GC-MS 

Internal Standard 

not specified 

not specified 

HPLC-DAD 

not specified 

Hexane 

Acetone 

Acetone 

Hexane 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Acetonitrile 

Spiking Tenax 

LC-MS/MS 

Internal Standard 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

External Standard 

Internal Standard 

Internal Standard 

External Standard 

Spiking Tenax 

LC-UV-VIS PDA 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking TNX 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

10.9 

not specified 

not specified 

not specified 

not specified 

5.3 

3.0 

8.9 

3.1 

28.6 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Spiking Tenax 

not specified 

Internal Standard 

-40- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 13. Bis(2-ethylhexyl) adipate values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0008 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

3.64 

2.10 

4.72 

3.48 

6.73 

3.50 

3.53 

3.84 

4.00 

4.43 

4.82 

8.83 

3.72 

4.58 

4.14 

4.29 

2.89 

3.88 

4.71 

4.50 

5.67 

1.91 

4.84 

3.84 

0.71 

3.54 

3.76 

4.40 

4.05 

2.07 

4.71 

3.64 

7.05 

3.50 

4.32 

3.87 

3.90 

4.61 

5.08 

8.82 

3.74 

4.63 

4.15 

4.43 

2.89 

3.89 

3.98 

4.60 

5.94 

2.18 

4.42 

4.08 

0.80 

3.66 

3.53 

4.20 

4.78 

2.12 

4.65 

3.69 

6.84 

3.87 

3.65 

3.72 

3.60 

4.62 

4.75 

8.47 

3.74 

4.82 

4.42 

5.19 

2.82 

4.14 

4.28 

4.50 

5.69 

1.91 

4.67 

3.98 

0.78 

4.00 

3.67 

4.20 

3.79 

2.10 

4.70 

3.41 

6.31 

3.88 

4.76 

3.78 

3.90 

4.47 

4.81 

8.67 

3.56 

4.69 

4.70 

5.07 

2.81 

3.81 

4.50 

4.90 

5.94 

2.10 

4.33 

3.89 

0.70 

3.88 

3.92 

4.60 

4.07 

2.10 

4.70 

3.56 

6.73 

3.69 

4.07 

3.80 

3.85 

4.53 

4.87 

8.70 

3.69 

4.68 

4.35 

4.74 

2.85 

3.93 

4.37 

4.63 

5.81 

2.02 

4.57 

3.95 

0.75 

3.77 

3.72 

4.35 

0.51 

0.02 

0.03 

0.13 

0.31 

0.22 

0.58 

0.07 

0.17 

0.10 

0.15 

0.17 

0.09 

0.10 

0.27 

0.45 

0.04 

0.14 

0.31 

0.19 

0.15 

0.14 

0.23 

0.10 

0.05 

0.21 

0.16 

0.19 

12.4 

1.0 

0.7 

3.7 

4.6 

5.9 

14.2 

1.8 

4.5 

2.1 

3.0 

1.9 

2.4 

2.2 

6.1 

9.5 

1.5 

3.7 

7.2 

4.1 

2.5 

6.7 

5.1 

2.6 

6.7 

5.5 

4.4 

4.4 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

not specified 

not specified 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-FID 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

not specified 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

External Standard 

Internal Standard 

Internal Standard 

Acetone 

Hexane 

Acetone 

Acetone 

Hexane 

Hexane 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

Internal Standard 

-41- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 14. Bis(2-ethylhexyl) phthalate values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0008 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

1.71 

1.69 

1.46 

2.23 

8.85 

1.275 

1.37 

1.35 

1.30 

1.96 

1.08 

1.11 

1.82 

1.44 

2.33 

8.92 

1.25 

1.48 

1.27 

1.50 

0.99 

1.07 

10.35 

11.02 

1.19 

1.41 

1.05 

1.48 

1.42 

1.62 

1.22 

2.03 

1.50 

2.289 

0.512 

1.924 

1.15 

0.23 

1.13 

1.58 

1.18 

1.37 

1.25 

1.71 

1.43 

1.50 

1.09 

1.85 

1.40 

2.193 

0.550 

1.875 

1.30 

0.14 

1.32 

1.57 

1.14 

1.38 

1.41 

2.33 

8.97 

1.30 

1.59 

1.47 

2.34 

8.64 

1.193 

1.162 

1.37 

1.30 

1.10 

1.28 

1.18 

9.40 

1.19 

1.37 

1.20 

1.50 

1.70 

1.42 

1.26 

1.92 

1.50 

2.266 

0.518 

1.961 

1.20 

0.24 

1.45 

1.58 

1.60 

1.28 

1.20 

1.49 

1.23 

8.84 

1.13 

1.48 

1.60 

1.66 

1.59 

1.56 

1.08 

1.91 

1.50 

2.023 

0.564 

1.894 

1.05 

0.56 

1.09 

1.64 

1.32 

1.62 

1.45 

2.31 

8.85 

1.22 

1.46 

1.30 

1.28 

1.43 

1.14 

9.90 

1.17 

1.41 

1.28 

1.59 

1.54 

1.53 

1.16 

1.93 

1.48 

2.19 

0.54 

1.91 

1.18 

0.29 

1.25 

1.59 

0.28 

0.19 

0.03 

0.05 

0.15 

0.05 

0.11 

0.03 

0.17 

0.41 

0.08 

0.97 

0.03 

0.05 

0.23 

0.11 

0.13 

0.09 

0.09 

0.07 

0.05 

0.12 

0.03 

0.04 

0.10 

0.18 

0.17 

0.03 

21.0 

11.5 

1.8 

2.2 

1.6 

4.2 

7.5 

2.7 

13.4 

28.6 

6.8 

9.8 

2.4 

3.7 

18.3 

7.2 

8.5 

5.6 

7.8 

3.9 

3.4 

5.5 

4.7 

2.0 

8.6 

62.9 

13.5 

2.0 

Acetone 

Hexane 

Acetone 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

GC-MS 

Internal Standard 

not specified 

not specified 

HPLC-DAD 

not specified 

Acetone 

Hexane 

Hexane 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

External Standard 

Internal Standard 

Internal Standard 

External Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

Standard Addition 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Hexane 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

-42- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 15. Caprolactam values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0010 

LC0013 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

10.10 

17.14 

8.15 

8.92 

11.21 

8.73 

9.52 

10.08 

9.32 

14.77 

9.45 

8.47 

6.35 

8.95 

9.62 

9.22 

8.35 

11.70 

10.30 

11.45 

3.85 

8.63 

8.57 

1.36 

21.31 

10.10 

9.60 

10.90 

17.94 

8.10 

9.34 

8.60 

8.55 

10.21 

10.07 

8.63 

14.81 

9.47 

9.39 

7.70 

9.38 

9.46 

9.02 

9.62 

11.70 

11.00 

11.70 

4.02 

7.80 

8.72 

1.33 

12.73 

10.70 

10.40 

10.80 

13.64 

8.10 

9.88 

10.40 

8.62 

9.39 

10.12 

8.67 

12.95 

9.40 

8.83 

7.25 

9.09 

9.20 

8.44 

9.81 

11.00 

11.90 

11.19 

3.70 

8.12 

8.29 

1.07 

20.10 

11.27 

10.10 

6.70 

12.88 

8.26 

8.98 

9.44 

8.94 

9.75 

10.34 

8.27 

12.71 

9.16 

8.41 

7.35 

9.68 

9.24 

7.82 

6.64 

11.80 

11.50 

9.31 

3.54 

8.06 

8.70 

1.07 

12.75 

11.91 

9.90 

9.63 

15.40 

8.15 

9.28 

9.91 

8.71 

9.72 

10.15 

8.72 

13.81 

9.37 

8.78 

7.16 

9.28 

9.38 

8.63 

8.61 

11.55 

11.18 

10.91 

3.78 

8.15 

8.57 

1.21 

16.72 

11.00 

10.00 

1.98 

2.51 

0.08 

0.44 

1.14 

0.17 

0.36 

0.13 

0.44 

1.14 

0.14 

0.45 

0.58 

0.32 

0.19 

0.63 

1.46 

0.37 

0.69 

1.09 

0.20 

0.35 

0.20 

0.16 

4.63 

0.77 

0.34 

20.6 

16.3 

0.9 

4.8 

11.5 

2.0 

3.7 

1.2 

5.0 

8.2 

1.5 

5.1 

8.0 

3.5 

2.1 

7.3 

17.0 

3.2 

6.2 

10.0 

5.4 

4.3 

2.3 

13.2 

27.7 

7.0 

3.4 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Acetone 

Hexane 

Acetone 

Spiking Tenax 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-FID 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

not specified 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Acetonitrile 

Spiking Tenax 

LC-MS/MS 

Internal Standard 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

External Standard 

Internal Standard 

Internal Standard 

External Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Spiking Tenax 

not specified 

Internal Standard 

-43- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 16. Dibutyl sebacate values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0008 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

5.00 

4.60 

5.04 

3.36 

5.07 

5.94 

7.00 

4.29 

3.20 

5.30 

4.77 

4.37 

5.20 

3.90 

4.41 

5.01 

4.42 

4.25 

5.32 

5.10 

5.74 

2.60 

5.56 

4.09 

0.83 

4.29 

4.12 

3.30 

4.54 

4.74 

5.05 

3.63 

7.38 

5.95 

6.10 

4.06 

3.40 

5.30 

4.60 

4.39 

5.12 

4.70 

5.28 

5.04 

4.41 

4.21 

4.00 

4.90 

5.91 

2.79 

5.30 

4.37 

1.07 

4.41 

3.96 

3.50 

4.94 

4.89 

5.22 

3.55 

7.28 

5.61 

7.35 

4.06 

3.50 

5.12 

4.24 

4.27 

5.25 

4.60 

4.17 

5.79 

4.24 

4.03 

4.14 

5.00 

5.66 

2.80 

5.50 

4.27 

1.06 

4.92 

3.69 

3.50 

4.12 

4.74 

4.98 

3.18 

6.16 

5.60 

7.91 

4.10 

4.00 

5.23 

4.70 

4.15 

5.24 

4.40 

5.50 

7.15 

4.12 

3.88 

4.72 

4.90 

5.97 

2.58 

5.30 

4.28 

0.89 

4.56 

4.00 

3.40 

4.65 

4.74 

5.07 

3.43 

6.47 

5.78 

7.09 

4.13 

3.53 

5.24 

4.58 

4.30 

5.20 

4.40 

4.84 

5.75 

4.30 

4.09 

4.55 

4.98 

5.82 

2.69 

5.41 

4.25 

0.96 

4.55 

3.94 

3.43 

0.41 

0.12 

0.10 

0.20 

1.09 

0.19 

0.76 

0.11 

0.34 

0.08 

0.24 

0.11 

0.06 

0.36 

0.65 

1.00 

0.14 

0.17 

0.60 

0.10 

0.14 

0.12 

0.13 

0.12 

0.12 

0.27 

0.18 

0.10 

8.8 

2.5 

2.0 

5.9 

16.8 

3.4 

10.7 

2.7 

9.7 

1.6 

5.1 

2.6 

1.1 

8.1 

13.4 

17.5 

3.4 

4.2 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

not specified 

not specified 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-FID 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

not specified 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

External Standard 

Acetone 

Hexane 

Acetone 

Acetone 

Hexane 

Hexane 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

13.3 

not specified 

not specified 

not specified 

not specified 

1.9 

2.5 

4.3 

2.5 

2.8 

12.6 

6.0 

4.6 

2.8 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Spiking Tenax 

not specified 

Internal Standard 

-44- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 17. 2,6-Diisopropylnaphthalene values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0050 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

1.71 

1.26 

1.53 

1.24 

1.79 

1.45 

1.30 

1.70 

1.35 

1.83 

4.23 

1.40 

1.32 

1.25 

1.32 

1.42 

1.21 

1.30 

1.54 

1.40 

2.41 

0.51 

0.34 

1.23 

0.30 

1.44 

1.24 

1.70 

1.79 

1.40 

1.58 

1.34 

2.02 

1.35 

1.30 

1.60 

1.36 

1.95 

4.29 

1.38 

1.36 

1.55 

1.51 

1.42 

1.25 

1.32 

1.39 

1.30 

2.40 

0.53 

0.85 

1.26 

0.26 

1.35 

1.22 

1.90 

1.87 

1.31 

1.52 

1.31 

1.94 

1.39 

1.31 

1.60 

1.35 

1.84 

3.28 

1.39 

1.35 

1.50 

1.62 

1.35 

1.18 

1.31 

1.47 

1.50 

2.30 

0.45 

0.91 

1.23 

0.28 

1.45 

1.14 

1.80 

1.21 

1.42 

1.52 

1.26 

1.83 

1.35 

1.34 

1.60 

1.35 

2.16 

4.07 

1.34 

1.30 

1.50 

1.70 

1.39 

1.14 

1.26 

1.47 

1.40 

2.45 

0.49 

0.92 

1.18 

0.26 

1.43 

1.13 

1.70 

1.65 

1.35 

1.54 

1.29 

1.90 

1.39 

1.31 

1.63 

1.35 

1.95 

3.97 

1.38 

1.33 

1.45 

1.54 

1.40 

1.20 

1.30 

1.47 

1.40 

2.39 

0.50 

0.76 

1.22 

0.28 

1.42 

1.18 

1.78 

0.30 

0.08 

0.03 

0.05 

0.10 

0.05 

0.02 

0.05 

0.01 

0.15 

0.47 

0.03 

0.03 

0.14 

0.16 

0.03 

0.05 

0.03 

0.06 

0.08 

0.06 

0.03 

0.28 

0.03 

0.02 

0.05 

0.06 

0.10 

18.1 

5.6 

1.9 

3.6 

5.5 

3.4 

1.4 

3.1 

0.4 

7.9 

11.8 

1.9 

2.1 

9.3 

10.7 

2.4 

3.9 

2.0 

4.2 

5.8 

2.7 

7.0 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

not specified 

not specified 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-FID 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

not specified 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

External Standard 

Internal Standard 

Internal Standard 

External Standard 

Acetone 

Hexane 

Acetone 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

36.8 

not specified 

not specified 

not specified 

not specified 

2.8 

7.0 

3.2 

4.7 

5.4 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Spiking Tenax 

not specified 

Internal Standard 

-45- 

 
 
 
EURL-FCM                                                                                                                                         ILC01-2014 Follow-up on food simulant E containing potential migrant substances 

Annex 18. 2-Ethyl-1-hexanol values reported by the participants. 

Lab Code 

Concentration (µg/g) 

Repetition 1 

Repetition 2 

Repetition 3 

Repetition 4 

Average 

SD 

RSD (%) 

Extraction 

Calibration 

Instrumentation 

Quantification 

LC0002 

LC0004 

LC0005 

LC0006 

LC0007 

LC0010 

LC0013 

LC0016 

LC0017 

LC0018 

LC0020 

LC0025 

LC0031 

LC0032 

LC0037 

LC0038 

LC0040 

LC0041 

LC0044 

LC0047 

LC0048 

LC0049 

LC0055 

LC0056 

LC0059 

LC0064 

LC0113 

11.00 

5.54 

6.70 

1.23 

11.43 

7.96 

10.04 

7.20 

9.24 

9.61 

12.22 

9.58 

7.45 

5.30 

6.09 

7.45 

7.28 

7.30 

7.51 

6.80 

13.62 

4.28 

6.70 

2.08 

9.72 

6.81 

8.50 

10.10 

6.62 

6.73 

1.12 

11.82 

8.09 

10.27 

8.30 

9.15 

9.58 

9.01 

9.63 

7.49 

5.65 

6.80 

7.06 

7.12 

7.92 

7.81 

8.20 

9.61 

4.24 

6.75 

1.23 

7.63 

7.85 

8.30 

11.00 

5.94 

6.70 

1.17 

13.69 

7.85 

9.77 

8.30 

9.21 

9.16 

10.11 

9.57 

7.54 

4.90 

6.56 

6.92 

6.56 

7.79 

7.82 

9.00 

9.26 

4.32 

6.88 

1.45 

10.82 

6.84 

8.40 

10.70 

6.67 

6.74 

1.28 

11.71 

7.87 

9.10 

7.40 

9.19 

9.81 

8.99 

9.10 

6.70 

6.35 

7.05 

6.13 

6.10 

8.15 

6.78 

7.90 

10.70 

6.19 

6.72 

1.20 

12.16 

7.94 

9.80 

7.80 

9.20 

9.54 

10.08 

9.47 

7.30 

5.55 

6.63 

6.89 

6.77 

7.79 

7.48 

7.98 

11.01 

10.87 

4.03 

6.63 

1.47 

9.38 

7.82 

8.60 

4.22 

6.74 

1.56 

9.39 

7.33 

8.45 

0.42 

0.55 

0.02 

0.07 

1.03 

0.11 

0.51 

0.58 

0.04 

0.27 

1.52 

0.25 

0.40 

0.62 

0.41 

0.55 

0.54 

0.36 

0.49 

0.91 

1.98 

0.13 

0.11 

0.36 

1.32 

0.58 

0.13 

4.0 

8.8 

0.3 

5.8 

8.5 

1.4 

5.2 

7.5 

0.4 

2.9 

15.1 

2.6 

5.5 

11.1 

6.2 

8.0 

8.0 

4.6 

6.5 

11.4 

18.2 

3.1 

1.6 

23.4 

14.1 

8.0 

1.5 

Spiking Tenax 

GC-MS 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

not specified 

not specified 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

Spiking Tenax 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-FID 

GC-FID 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

not specified 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

External Standard 

Internal Standard 

Internal Standard 

External Standard 

Hexane 

Hexane 

Acetone 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Hexane 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Acetonitrile 

Standard Solution 

Hexane 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

not specified 

not specified 

not specified 

not specified 

Acetone 

Acetone 

Acetone 

Acetone 

Acetone 

Hexane 

Acetone 

Acetone 

Spiking Tenax 

Standard Solution 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Spiking Tenax 

GC-MS/GC-FID 

Internal Standard 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

Spiking Tenax 

GC-MS 

GC-MS 

GC-MS 

GC-MS 

Internal Standard 

Internal Standard 

Internal Standard 

Internal Standard 

Spiking Tenax 

not specified 

Internal Standard 

-46- 

 
 
 
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European Commission 
EUR 27166 EN – Joint Research Centre – Institute for Health and Consumer Protection 

Title: Report of an Inter-laboratory Comparison from the European Union Reference Laboratory for Food Contact Materials 
        ILC01-2014 – Follow-up ILC01-2013 on Proficiency Testing on Food Simulant E containing a cocktail of potential migrant substances  

Authors: Juliana Silva Félix and Catherine Simoneau 

Luxembourg: Publications Office of the European Union 

2015 – 48 pp. – 21.0 x 29.7 cm 

EUR – Scientific and Technical Research series – ISSN 1831-9424 
ISBN 978-92-79-47122-3 

doi:10.2788/455286 

L
B
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N
A
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2
7
1
6
6
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E
N
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N

JRC Mission 

As the Commission’s  
in-house science service,  
the Joint Research Centre’s 
mission is to provide EU  
policies with independent,  
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and technical support  
throughout the whole  
policy cycle. 

Working in close  
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through developing  
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and standards, and sharing 
its know-how with  
the Member States,  
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and international partners. 

Serving society  
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doi:10.2788/455286 

ISBN 978-92-79-47122-3