ICS. 71.100.40  
Y 43  
 
GB 
 
National Standards of the People’s Republic of China  
 
GB XXXX - XXXX  
 
 
 
 
 
Humectants for Toothpastes    Glycerine and Macrogol  
 
 
 
 
(Draft for Approval)  
(Draft Completion Date: 1 August 2007)  
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
Issue Date: XXXX – XX -XX             Implementation Date: XXXX –XX -XX 
 
 
Issued by General Administration of Quality Supervision, Inspection and 
Quarantine of the People’s Republic of China and Standard Administration of 
the People’s Republic of China     
 
Preface  
 
The content hi ghlighted in bold characters in Table 1 and Table 2 of this 
standard is mandatory while the rest is recommended.  
 
This standard is compiled in reference to the US Pharmacopoeia (USP30/NF25) and 
integrated with regards to the particular situation of our to othpaste industry.  
 
This standard is proposed by China Light Industry Association.  
 
This standard is under the jurisdiction of National Toothpaste and Wax Product 
Standardisation Centre.  
 
The main drafting organisations of this standard include: National Light Industry 
Toothpaste and Wax Product Quality Supervision and Test Centre, Beijing Procter & 
Gamble Technology Co. Ltd, Liuzhou LMZ Co., Ltd, Masson Group Co. Ltd, 
Shanghai Toothpaste Factory of Shanghai White Cat Co. Ltd, Chongqing Dencare  
Oral Care C o., Ltd, Guangzhou Colgate -Palmolive Co. Ltd, Unilever (China) Co. Ltd.  
 
The main drafters of this standard were: Zou Bin, Ye Tingting and Ma Xuan.  
 
This standard was issued on ... for the first time.  
 
    
 
Humectants for toothpastes    Glycerine and macrogo l 
 
1 Scope  
 
This standard sets the requirements, test methods, and rules for the inspection, 
packaging, labelling, transportation and storage of glycerine and macrogol in the 
humectants used in toothpaste.  
 
This standard is applicable to glycerine and macrog ol humectants used in toothpaste.  
 
2 Normative References  
 
The provisions of the following documents become provisions of this standard after 
being referenced. For dated reference documents, all later amendments (excluding 
corrigenda) and versions do not app ly to this standard; however, the parties to the 
agreement are encouraged to study whether the latest versions of these documents are 
applicable. For undated reference documents, the latest versions apply to this standard.  
 
GB/T 191 -2000  Packaging - Pictor ial Marking for Handling of Goods  
GB/T 601  Chemical Reagent - Preparations of Standard Volumetric Solutions  
GB/T 602  Chemical Reagent - Preparations of Standard Solutions for 
Impurity  
GB/T 603  Chemical Reagent - Preparations of Reagent Solutions for use  in 
Test Methods  
GB/T 6682  Water for Analytical Laboratory Use - Specification and Test 
Methods  
GB/T 6678  General Principles for Sampling Chemical Products  
GB/T 13216.2 – 1991  Test Methods for Glycerines - Determination of Transparency  
GB/T 13216.3 –1991  Test Methods for Glycerines - Determination of Odour  
GB/T 13216.4 –1991  Test Methods for Glycerines - Determination of Colour (Hazen 
Unit-Platinum -Cobalt Scale)  
GB/T 13216.5 –1991  Test methods for Glycerines - Determination of Density at 
20ºC  
GB/T 13216.6  –1991  Test Methods for Glycerines - Determination of Glycerol 
Content  
GB/T 13216.7 –1991  Test Methods for Glycerines - Limit Test for Chloride  
GB/T 13216.8 –1991  Test methods for Glycerines - Determination of Sulphated Ash 
- Gravimetric Method  
GB/T 13216. 9 – 1991  Test methods for Glycerines - Determination of Acidity or 
Alkalinity - Titrimetric Method  
GB/T 13216.10 – 1991 Test methods for Glycerines - Determination of 
Saponification Equivalent  
GB/T 13216.13 – 1991 Test methods for Glycerines - Test of Redu cing Substances  
JJF1070 —2005   Rules of Metrological Testing for Net Quantity of Products in Pre -
packages with Fixed Content  
 Decree No 75 of the General Administration of Quality 
Supervision, Inspection and Quarantine of the People’s Republic of    
China, Pro mulgating the Measures for Administration of 
Measurement and Supervision of Pre -packed Commodities  
 Pharmacopoeia of the People’s Republic of China, 2005  Edition 
(Part Two)  
 
3 Requirements  
 
3.1 Glycerine  
The sensory characters, physical and chemical elements and  the limits of toxic 
substances of glycerine should meet the requirements set out in Table 1.  
 
Table 1  
Character  Item Saponification  Zymotechnics  
Appearance (transparency)  Transparent, no suspended substance or 
sedimentation  
Smell  No odd odour  Sensory 
Character  
Colour (hazen)                                 30 20 
Glycerine content / %                       98.0 95.0 
Density (20 ) / (g/ml)                      1.2559  1.2481  
Chloride (calculated by C1)              0.01 0.001  
Sulphated ash / %                              0.01 
Acidity or alkalinity / (mmol/100g)  0.01 
Reducing substance  No sedimentation or 
silver mirror reaction  - 
Saponification equivalent / 
(mmol/100g)  1.0 - Physical 
& 
Chemical 
Character  
Molysite (calculate by Fe) (mg/kg)   - 2 
Diglycol and rela ted compounds % 
 1.0 (total of diglycol and related impurities, 
other impurities  0.1 respectively)  
Heavy metal content (calculate by 
Pb) / (mg/kg)                                      5 Limits of 
Toxic 
Substance  Arsenic content (calculated by As) / 
(mg/kg)                                              2 
 
3.2 Macrogol  
The sensory characters, physical and chemical elements and the limits of toxic 
substances of macrogol should meet the requirements set out in Table 2.  
 
Table 2  
Item Character  
Sensory Character  Appearance  No colour  or near colourless, clear 
viscous fluid, or semi clear soft wax, or 
white solid wax flakes or granular power  
Average molecular weight  200 to 8000  
pH 4.0 to 7.5  Physical & 
Chemical Elements  Burning residue %  0.2 
Diglycol and  glycol %  0.25 (total of two)  
Heavy metal (calculated by lead) ) 
(mg/kg)                                          5 Limits of Toxic 
Substance  
Arsenic / (mg/kg)  3 
 
 
3.3 Net Content  
The net content of packaged humectants in toothpastes should conform to the    
requirements stipulated in JJF1070 –2005 . 
 
4 Test Methods  
With the exception of any special requirements, the reagents and water of this 
stand ard are all pure analytic reagents and water that conform with the stipulations 
of GB/T6682.  
 
With the exception of any special requirements, the standard solution for the 
titration analysis, the standard solution for the impurity measurement and for the 
preparation and products used the test in this standard are all prepared according 
to the provisions of GB/T601, GB/T602 and GB/T603.  
 
4.1 Test Methods for Glycerine in Toothpaste  
 
4.1.1 Appearance  
Test according to the provisions of GB/T 13216.2.  
 
4.1.2 Odour  
Test accord ing to the provisions of GB/T 13216.3.  
 
4.1.3 Colour  
Test according to the provisions of GB/T 13216.4.  
 
4.1.4 Glycerine Content  
Test according to the provisions of GB/T 13216.6.  
 
4.1.5 Density  
Test according to the provisions of GB/T 13216.5.  
 
4.1.6 Chloride  
Test according to the  provisions of GB/T 13216.7.  
 
4.1.7 Sulphated Ash  
Test according to the provisions of GB/T 13216.8.  
 
4.1.8 Acidity or Alkalinity  
Be tested according to the provisions of GB/T 13216.9.  
 
4.1.9 Reducing Substance  
Be tested according to the provisions of GB/T 13216.13.  
 
4.1.10  Saponif ication Equivalent  
Be tested according to the provisions of GB/T 13216.10.  
 
4.1.11  Molysite  
Test according to the provisions of Appendix VIIIG to Pharmacopoeia of the 
People’s Republic of China, 2005 Edition (Part Two).  
 
4.1.12  Diglycol and Related Compounds  
    
4.1.12.1  Apparatus  
Gas phase chromatography: with a flame ionisation detector, chromatographic 
column G43 (6% cyanopropylphenyl, 94% p -methylpolysiloxane - substance 
quantity in percentage ) (0.53 mm × 30m × 3  m) as the fused silica capillary 
column, sample entry lining tube type as inward warping cup. 
Chromatography settings as follows: initial chromatographic column 
temperature of 100 ºC; after injecting the sample increase the temperatur e to 
220ºC at a speed of 7.5  /min and maintain for 4 min. Maintain a temperature 
of 220 ºC at the sample entry area and maintain the temperature of the detector 
at 250 ºC. Use helium as carrier gas. Diversion ratio as 10:1, linear speed: 38 
cm / s. After en try of the resolution fluid, record the peak chromatogram 
response according to the specified conditions of the test method. The 
separation of the two peaks between the diglycol and glycerine should not be 
less than 7.0. Repeat by injecting the standard so lution, and record the 
chromatographic peak area. The relative deviation to the standard should not 
exceed 15%.  
 
4.1.12.2  Reagent  
a) Glycerine and glycol: chromatographic pure;  
b) Resolution fluid: weigh the chromatographic pure diglycol and glycerine 
accurately, dissolv e them in water, diluting them quant itatively - step by 
step diluting if necessary - and create diglycol and glycerine solutions with 
a concentration of around 0.5 mg / ml;  
c) Standard solution: weigh the chromatographic pure diglycol accurately, 
dissolving i t in water, diluting it quantit atively - step by step diluting if 
necessary - and create a diglycol solution with a concentration of around 
0.05 mg / ml;  
d) Testing solution: accurately add 5g of glycerine in a 100 ml measuring 
flask, dilute with water to the  scale and shake it evenly.  
 
4.1.12.3  Test procedure  
Conduct the test with the same volume (about 0.5  L) of the standard solution 
and test the solution respectively. Record the chromatograms and measure the 
peak area. Calculate the diglycol content (C 1) in the gl ycerine sample using 
the formula (1):  
  
  
In the formula:  
C1 – diglycol content, %;  
Cs – diglycol concentration in the standard solution, unit as mg/ml;  
Cu – diglycol concentration in the testing solution, unit as mg/ml;  
ru – chromatograph peak area of di glycol in the testing solution;  
rs - chromatograph peak area of diglycol in the standard solution.  
 
Calculate the other impurity (without the solution peak) content (C 2) in the 
glycerine sample using the formula (2):  
    
  
  
In the formula:  
C2 – impurity (wit hout the solution peak) content in the glycerine sample, %;  
ri – peak area of each impurity in the tested solution;  
rs – total peak areas measured from the test solution.  
 
4.1.13  Arsenic  
Test according to the provisions on the s ilver diethyldithiocarbamate 
spectr ophotometric method  of Appendix VIIIJ to the Pharmacopoeia of the 
People’s Republic of China, 2005 Edition (Part Two).  
 
4.1.14  Heavy Metal  
Test according to the provisions on the first method  of Appendix VIIIH to the 
Pharmacopoeia of the People’s Republic of Chin a, 2005 Edition (Part Two).  
 
4.2 Macrogol  
 
4.2.1 Appearance  
Test according to the provisions regarding Macrogol set out in the 
Pharmacopoeia of the People’s Republic of China, 2005 Edition (Part Two).  
 
4.2.2 Average Molecular Weight  
 
4.2.2.1  Main Apparatus  
Heat resistance pressu re bottle  
 
4.2.2.2  Reagent  
a) Phthalic anhydride solution: place 49.0g phthalic anhydride in a brown 
bottle, dissolve it in 300 ml distilled pyridine or 300 ml pyridine from a 
newly opened bottle, fully oscillate until it completely dissolves. Add 7g 
imidasole, caref ully shake to dissolve and leave for 16 hours before use.  
b) Macrogol testing solution: carefully place 25.0 ml phthalic anhydride 
solution into a dry heat resistance pressure bottle. Add an accurately 
weighed sample of macrogol with the mass of its expected average 
molecular weight at around 1/160. Wrap the pressure bottle tightly with a 
cloth.  
c) Sodium hydroxide: 0.5 mol/l.  
 
4.2.2.3  Test Procedure  
Immerge the bottle in a 96ºC -100ºC water bath; the immerging depth of the 
bottle should be at fluid level in the pressure bottle. Remove the bottle after 5 
minutes and shake it evenly without unwrapping the cloth. Continue to heat 
the water bath for 30 minutes then remove it, allowing it to cool to room 
temperature. Remove the pressure bottle from the cloth bag, carefully ope ning 
the cap to release the pressure, add 10 ml water and shake thoroughly. Leave 
for 2 minutes and add 0.5 ml phenolphthalein. With 1 +100 pyridine solution, 
titrate with 0.5 mol/l sodium hydroxide until a sustained pink colour initially 
appears for 15 se conds. Record the consumption of the titration liquid volume    
as S. Using the same method, carry out a blank test in 25.0ml phthalic 
anhydride solution and pyridine, recording the volume of consuming 0.5 mol / 
L of sodium hydroxide as B.  
 
4.2.2.4  Average Molecular Weight Calculation  
Calculate the average molecular weight (M) of macrogol using the formula (3):  
 
  
  
In the formula:  
M – average molecular weight of macrogol;  
W – macrogol mass of the prepared testing solution, unit as g;  
B – blank consuming 0.5 mol/l sod ium hydroxide, unit as ml;  
S – sample consuming 0.5 mol/l sodium hydroxide, unit as ml;  
N – molar concentration of the sodium hydroxide solution, unit as mol/L.  
 
4.2.3 pH 
Tested according to the provisions stipulated in Appendix VIH to the 
Pharmacopoeia of the P eople’s Republic of China, 2005 Edition (Part Two).  
 
4.2.4 Diglycol and Glycol  
 
4.2.4.1  Diglycol and glycol measurement of the macrogol sample with an average 
molecular weight of less than 450  
 
4.2.4.1.1  Main Apparatus  
Gas phase chromatography: with a flame ionisation detector, t he 3mm × 1.5m 
stainless steel chromatographic column filled with untreated diatomite bearing 
12% sorbitol. Use nitrogen as the carrier gas or another suitable inert gas with 
a flow rate of 50 ml/min. The column temperature should be maintained at 140 
ºC. M aintain the sample entrance at 250ºC and the flame ionisation detector 
temperature at 280ºC.  
 
4.2.4.1.2  Reagent  
a) Diglycol and glycol: chromatographic pure;  
b) Standard solution: make up the standard solution with chromatographic 
pure diglycol and glycol both with a conc entration of 500  g / ml;  
c) Testing the solution: place the accurately weighed 4g macrogol into a 10 
ml measuring flask; dilute it to the scale and shake evenly.  
 
4.2.4.1.3  Test Procedure  
Add 2.0 ml standard liquid sample, record its chromatogram and adjust 
operatin g conditions so as to make the peak height not less than 100 mm. 
Measure the first chromatographic peak height (glycol) and the second peak 
height (diglycol) and record as P1 and P2 respectively. Put in 2.0  L testing 
solution sample, record its chromatog ram in the same operating condition. 
Measure the first chromatographic peak height (glycol) and the second peak 
height (diglycol) and record as p1 and p2 respectively.  
    
4.2.4.1.4  Calculation of Diglycol and Glycol  
The glycol content in the sample (C 3) is calculated using the formula (4):  
 
  
  
In the formula:  
C3 – glycol content, %;  
c1 – glycol concentration of the standard solution, unit as mg / ml;  
p1 – glycol peak height of the testing solution, unit as mm;  
P1 - glycol peak height of the standard solution, unit as mm; 
W – glycol mass used in the test, unit as mg.  
 
The diglycol content in the sample (C 4) is calculated using the formula (5):  
 
  
  
In the formula:  
C4 – diglycol content, %;  
c2 – diglycol concentration of the standard solution, unit as  g / ml;  
p2 – diglycol peak height of the testing solution, unit as mm;  
P2 - diglycol peak height of the standard solution, unit as mm;  
W – diglycol mass used in the test, unit as mg.  
 
4.2.4.2  Diglycol and glycol measurement of the macrogol sample with average 
molecular weight of higher than 450 and lower than 1000  
 
4.2.4.2.1  Main Apparatus:  
a) distillation flask;  
b) spectrophotometer.  
 
4.2.4.2.2  Reagent:  
a) nitrate: 0.25 mol/l;  
b) ceric ammonium nitrate: dissolve 6.25g ceric ammonium nitrate in 100 ml 
0.25 mol/l nitrate solution and use within three days;  
c) standard solution: place 62.5 mg diglycol in a  25 ml measuring flask. 
Dissolve the diglycol by the solution, which is mixed by the same 
voluminal newly -distilled acetonitrile and water, and then dilute the 
solution to scale;  
d) testing solution: dissolve 50.0g macrogol into 75 ml diphenyl ether in a 
250 ml distillation flask. If any crystallisation occurs, preheat the solution 
to dissolve the crystals. Slowly distil under a pressure of 1 -2 mm mercury 
column; collect the distillation in a 100 ml co ntainer with 1 ml graduation 
until the distillation reaches 25 ml. Add 20.0 ml water into the distillation, 
fully oscillate, and then keep still for delamination. Place the mixture in an 
ice bath to solidify the diphenyl ether and separate the two -phase so lid-
liquid. Filter the separated water layer and collect the filtrate. Wash the 
diphenyl ether with 5.0 ml ice water, filter and collect the washing fluid. 
Mix the filtrate and washing fluid in a 25 ml conical flask and add water to    
dilute to the scale, an d then shake evenly. Heat the solution to room 
temperature, if necessary. Mix this solution evenly with 25.0 ml newly 
distilled acetonitrile in a 125 ml conical flask with a glass plug.  
 
4.2.4.2.3  Test Procedure  
Separately place 10.0 ml standard solution and 10.0 ml  testing solution into 
two 50 ml flasks with 15.0 ml ceric ammonium nitrate solution in each and 
mix evenly. Within 2 to 5 minutes use 1 cm cells and spectrophotometers with 
a maximum absorption wavelength of 450 nm to simultaneously measure the 
absorbency  of the two solutions. Blank contrast 15.0 ml ceric ammonium 
nitrate solution and 10.0 ml mixture solution with the same voluminal newly 
distilled acetonitrile and water. The absorbency of the testing solution should 
not exceed the absorbency of the standa rd solution, i.e. the total content of the 
glycol and diglycol should not exceed 0.25%.  
 
4.2.5 Burning Residue  
Test according to the provisions set out in Appendix VIIIN to the 
Pharmacopoeia of the People’s Republic of China, 2005 Edition (Part Two).  
 
4.2.6 Heavy Met al 
Test according to the provisions set out in the first method  of Appendix VIIIH 
to the Pharmacopoeia of the People’s Republic of China, 2005 Edition (Part 
Two).  
 
4.2.7 Arsenic  
Test according to the provisions on silver diethyldithiocarbamate 
spectrophotometric  method set out in Appendix VIIIJ to the Pharmacopoeia of 
the People’s Republic of China, 2005 Edition (Part Two).  
 
4.3 Net Content  
The net content of packaged humectants for toothpaste should be tested 
according to the provisions stipulated in  JJF1070 -2005.  
 
5 Inspection Rules  
 
5.1 Inspection Classification  
 
5.1.1 Final Factory Inspection  
Items inspected in the final factory inspection for glycerine are sensory 
characters, physical and chemical elements and requirements for “diglycol and 
related compounds”.  
 
Items inspected in the final factory inspection for macrogol are sensory 
characters, physical and chemical elements and requirements for “diglycol and 
glycol”.  
 
5.1.2 Type Inspection  
All items specified in the technical requirements of this standard are type 
inspection items. A type inspection should be conducted every three months    
under normal conditions. A type inspection must be carried out if one of the 
following conditions occur:  
a) modification made to a key production process;  
b) modification made to main raw ma terials;  
c) production resumed after a suspension;  
d) if required by national quality supervision authorities or buyers.  
 
5.1.3 Acceptance Inspection  
The buyer is entitled to perform an acceptance inspection on the received 
goods according the relevant terms of the co ntract signed by the supplier and 
buyer and in accordance with the provisions set out in this standard. The 
acceptance inspection should be carried out within 15 days from the date of 
delivery.  
 
5.2 Batching and Sampling Rules  
 
5.2.1 Products of the same specificati on supplied in one delivery are considered as 
one batch.  
 
5.2.2 A product may only be released from the factory after being inspected by the 
quality control department of the production enterprise in accordance with this 
standard and when issued with an inspect ion report; the recipient also 
conducts an acceptance inspection in accordance with this standard.  
 
5.2.3 Sampling of glycerine and macrogol should be conducted according to 
GB/6678 and the sample quantity should not weigh less than 500g.  
 
5.3 Determination Rules  
If the test result does not meet the requirements of the standard, new samples 
should be taken and the test should be repeated. If the repeated test result still 
does not meet the requirements, the entire batch of the product shall be 
considered as unqualifi ed. 
 
5.4 Archiving Sample and Sample Preserving  
In each batch of inspected products a sample should be preserved for 30 days 
as an archiving sample.  
 
6 Packaging, Labelling, Transportation and Storage  
 
6.1 Packaging  
 
As a kind of oral product with a high level of cl eanness, it should be ensured 
that the container of this product is clean, and inside coated steel barrels, 
polyethylene plastic buckets, square polyethylene plastic cans, containers with 
polyethylene plastic lining, galvanised buckets, stainless steel buc kets or 
tankers could be selected as the packaging.  
 
 Packaging should conform to the provisions set out in GB 191.  
 
6.2 Labelling     
The contents of the packaged product should be clearly labelled with the 
product name, name and address of the manufacturer, trad e mark, production 
batch or production date, shelf life and serial numbers of applied standards.  
 
6.3 Transportation  
This product should not be transported together with any toxic or harmful 
substances, and should be loaded and unloaded with care so as to avoi d 
causing deformation or rupture to the packaging.  
 
6.4 Storage  
This product should be stored in a dry and ventilated store; it should not be 
stored outdoors; should avoid being stored where dust and water may be 
collected on the package; and should not be sto red together with any toxic, 
harmful or contaminating goods, and a ‘first come, first go’ principle should 
be applied in the store so as to cut the storage time down to as short a length as 
possible.  
 
 
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