Focusing Review

CHROMATOGRAPHY, Vol.34 No.1 (2013)

Focusing Review

Sample Preparation of Volatile Organic Compounds with
Needle−Type Extraction Device
Ikuo Ueta＊
Department of Applied Chemistry, University of Yamanashi
4−3−11 Takeda, Kofu 400−8511, Japan.

Abstract
Needle−type extraction devices have been developed for the simple and sensitive determination of gaseous volatile organic compounds(VOCs) in gas chromatography (GC). The needle−type extraction device allows direct insertion of the extraction medium into the GC injection port, therefore, simple and rapid desorption of the extracted analytes could be achieved. For simultaneous derivatization and preconcentration of VOCs, fiber−packed needle was developed. The fiber−packed needle was prepared with a bundle of fine filaments typically coatedwith methyl−polysiloxane. During the extraction, target analytes, such as volatile aldehydes or ethylene oxide, were simultaneously derivatized and concentrated in the extraction needle.
Particle−packed needle has been developed for the extraction of VOCs commonly found in environmental gaseous samples. Several particulate materials, such as porous polymer particles or activated carbon, were employed as the extraction media for the respective target analytes.
The particle−packed extraction needle was successfully applied for various analytical situations, such as in−door air analysis, fire investigation and human breath analysis.
Keywords : Sample preparation, VOCs, Extraction, Needle, Gas chromatography

employed for the concentration of VOCs in air samples, i.e., sol-

1. Introduction
Quantification of volatile organic compounds (VOCs) in envi-

vent desorption and thermal desorption (TD) methods. The solventronmental air has been recently focused because of their adverse

desorption method showed relatively low sensitivity, and the sol-

effects on human health, including the so−called multiple chemicalvent peak can often interferes some analytes in the chromatogram.

sensitivity and sick building syndrome [1,2]. To investigate the ef-

The TD is a solvent−free technique and has a high sensitivity, how-

fect of VOCs on human health and prevent the above illnesses, aever, it requires a relatively expensive, specially−designed desorp-

sensitive and reliable method for determining the VOCs in air sam-tion instrument.

ples is desired. For the determination of gaseous VOCs, the analy-

Solid−phase microextraction (SPME) is one of the most ad-

sis in gas chromatography (GC) is one of the most promising meth-vanced sampling techniques for typical VOCs analysis in GC, andods, because of its selectivity and sensitivity, as well as wide avail-it has several attractive features over other traditional sample

ability [3,4]. However, a sample preconcentration process should

preparation techniques [5]. However, most of the SPME techniques

still be needed for an accurate and precise determination of theseare based on static sampling, therefore, a relatively long extraction

VOCs.

time is needed to obtain a satisfactory sensitivity. As an alternative
to the active extraction of VOCs, the use of needle−type extraction

Typically, two types of sample preparation methods have been
Corresponding author: Ikuo Ueta
Tel: +81−55−220−8552
Fax: +81−55−220−8547
E−mail address: iueta@yamanashi.ac.jp―２３―

CHROMATOGRAPHY, Vol.34 No.1 (2013)

2. Fiber−packed needle for simultaneous derivatization/precon-

devices has been recognized to be an effective sample preparation

centration of VOCs

technique [6,7]. Compared to the conventional SPME, the needle−

The fiber−packed extraction needle was designed for the deri-type sampling device has been regarded to have a good mechanicalvatization and concentration of VOCs, such as volatile aldehydes,

strength and also a high extraction capacity.
In our previous investigations, the authors developed miniatur-

ketones and ethylene oxide (EO). Illustration of the fiber−packed

ized needle−type extraction devices for rapid and sensitive determi-

needle was shown in Fig. 1A. In the fiber−packed needle, a bundle

nation of gaseous VOCs in GC [8−10]. The needle−type extractionof Zylon filaments was packed, because of their excellent thermal

devices were prepared with an extraction sorbent in a specially−de-stability and also their high−resistance to typical organic solvents

signed stainless steel needle. The target analytes are extracted on
the sorbent when a gaseous sample is passed through the packed
sorbent section in the needle. The extracted analytes can then be
thermally desorbed in the heated GC injection port [11−17]. This
technique does not require any additional desorption instrument
and/or cryogenic focusing process. Therefore, the extraction employing a needle−type device can be regarded as a simple, rapid,
and useful extraction/sample preparation method, and actually, several applications have already been reported for the determinationof trace level of VOCs in gaseous samples.
In this review, simultaneous derivatization/preconcentration of
VOCs using a fiber−packed extraction needle is described [18,19].
The determination of typical VOCs with a particle−packed extraction needle [20] and its applications for several analytical situations
are also reviewed [21−25].
Fig. 1 Schematic illustration of needle−type extraction devices. (A)Fiber−packed needle and (B) particle−packed needle.

Fig. 2 Schematic diagram of the extraction/derivatization and desorption of analytes using fiber−packed needle.
Modified from Fig. 4 in reference 18 with permission.

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Ikuo Ueta[26,27]. The surface of the filament was coated with an HR−1 material (100%−methyl−polysiloxane; Shinwa Chemical Industries,
Kyoto, Japan). To prepare the fiber−packed needle, a 4 cm of thepolymer−coated filaments (415 filaments) was folded in half, andthen packed into the needle (85 mm×0.5 mm I.D., 0.7 mm O.D.).
The resulting a section of about 20 mm in length (830 filaments)
was packed with the filaments, and one end of the packed section
was positioned just before the side hole of the needle. Approximately 8 min of the extraction time was required for the extractionof 50 mL of gaseous sample with the needle. The derivatized analytes were determined by gas chromatography−mass spectrometry(GC−MS). The scheme for the extraction of the air sample and thedesorption of the analytes using the fiber−packed needle is illustrated in Fig. 2.
2.1. Determination of volatile aldehydes and ketones
For the determination of volatile aldehydes and ketones in air
samples, 2,4−dinitrophenylhydrazine (DNPH) was employed as thederivatization reagent [28]. Prior to the introduction of the sample
gas into the fiber−packed needle, as illustrated in Fig. 2, the DNPH
solution of approximately 50 µL (0.1 mg/mL in acetonitrile) was
pumped through the needle, and then the remaining solution wasFig. 3 Chromatograms for the separation of DNPH derivatives of(A) aldehydes and (B) ketones in programmed SIM mode. Sample
concentration: Formaldehyde (FA), 25 ng/L; acetaldehyde (AA),
300 ng/L; propionaldehyde (PA), 400 ng/L; acetone, 500 ng/L and
MEK, 600 ng/L. GC conditions: column, DB−1 fused−silica capillary (15 m×0.25 mm I.D., film thickness 0.25 µm); temperature
program, A 150oC (1.0 min) to 230oC at 10oC/min and B 150oC (1.0min) to 230oC at 10oC/min; column head pressure, He 80 kPa.
Modified from Fig. 8 in reference 18 with permission.

vented by pumping 1 mL of N2 through the needle. Next, the needle was attached to a commercially−available vacuum gas sampling device. Reacted with DNPH in the needle, aldehydes and ketones in the air samples were derivatized to be the corresponding
hydrazones, and simultaneously extracted in the extraction needle.
After the derivatization/extraction process, the needle was attached
to an injection syringe containing acetonitrile and N2 gas, and inserted into the GC injector. Desorption and injection were performed simultaneously by injecting acetonitrile and N2 through theneedle at the heated injector, as shown in Fig. 2. Injection was per-Table 1. LODs and LOQ for aldehydes, ketones and EO using fiber

formed immediately after the insertion of the needle into the injec-−packed needle.

tor, because it was found in the preliminary experiments that no

Analytepreheating time was necessary for an effective desorption under theFormaldehyde
Acetaldehyde
Propionaldehyde
AcetoneEO

optimized desorption conditions.
The extraction performance was evaluated based on the optimized volume of the desorption solvent and the desorption temperature, where a practically complete desorption (more than

LOD(ng/L)

LOQ(ng/L)

1.2
3.6
4.7
11.7
1.8

3.6
10.8
14.1
35.1
5.4

99.99%) at the first desorption. Typical chromatogram for the separation of aldehydes sample with time−programmed SIM monitor-

In order to evaluate the storage performance of the fiber−packed

ing is shown in Fig. 3A. In Fig. 3B, separation of acetone andneedle, the sampled needles were stored at room temperature, at

methyl ethyl ketone (MEK) is also presented. The limit of detec-

about 24 oC, for up to 3 days after the sampling. During this storagetion (LOD) and limit of quantification (LOQ) of the proposed

period, all of the needles were sealed with a set of cap and plug in-method was summarized in Table 1. Taking into account the sam-

dividually manufactured from a small piece of polytetrafluoroeth-

pled gas volume of 50 mL and the concentration range found in

ylene (PTFE). The results demonstrated an excellent storage per-typical in−house air measurements, the data in Table 1 clearly

formance of the fiber−packed needle. The extracted samples could

demonstrate a practical quantification level for these compounds.

be almost quantitatively determined after the storage period, which―２５―CHROMATOGRAPHY, Vol.34 No.1 (2013)

3.1. Determination of tobacco−related VOCs

is an additional advantageous feature, especially for a large number

Three smoking−related samples, i.e., side stream, main streamof samples were extracted on−site at the same time [20].
An alternative derivatization reaction of carbonyl compounds

and smoker’s breath, were collected in gas sampling bags, and a 50

with O −(2,3,4,5,6−pentafluorobenzyl)hydroxylamine hydrochlo-mL portion of each sample was extracted by MA/EGDMA particle

ride (PFBHA) was also successfully introduced. On the basis of the−packed needle followed by the analysis in gas chromatography−

preliminary derivatization experiments in the polymer−coated fiber

flame ionization detection (GC−FID). Compared to the side−packed needle device, an aqueous solution of PFBHA (10 mg/

stream, nicotine in the main stream seemed to be eliminated mainlymL) was used as the derivatization reaction. For the desorption ofby the tobacco filter, however, as expected, it still contained vari-

PFBHA derivatives, pure water (30 µL) and N2 gas were used. For-ous types of organic compounds. In addition, a significantly lower

maldehyde and acetaldehyde in a smoker’s breath sample werelevel of organic compounds in smoker’s breath was confirmed.

measured with both DNPH and PFBHA derivatization methods us-

One can conclude from above comparison that most of the VOCs

ing the same fiber−packed needle, and these quantitative results

generated during the smoking might remain trapped in their respi-

could have a good agreement [21].

ratory system [21].
In recent years, a new smoking hazard has been reported, so−called “third−hand smokin” [29]. This is residual tobacco smoke

2.2. Sample preparation of EO
As an extension to the above studies, the fiber−packed needle

pollution, which occurs after smoking. The MA/EGDMA particle−

was further applied to a rapid and sensitive determination of gase-packed extraction needle was applied to the evaluation of a poten-

ous EO. An aqueous solution of HBr was used for the derivatiza-

tial risk of third−hand smoking. Five different types of fabrics weretion of EO. In the needle, EO was successfully reacting with HBr

exposed to side−stream smoke, and VOCs desorbed from the eachto form 2−bromoethanol at room temperature. The derivatized ana-

fabric samples were determined (Fig. 4). Significantly higher con-lyte was desorbed by passing a small amount of methanol in thecentrations for ammonia and 2−furaldehyde (data not shown) wereneedle. The LOD and LOQ of EO in this method were summarized

observed for the cotton and linen fabric, however, higher concen-

in Table 1. Satisfactory storage performance for 3 days at room

trations for other smoking−related aromatic VOCs were obtained

temperature was also confirmed. Taking advantage of the rapid re-with the acetate fabric. Although a more extensive study, including

action with HBr in the fiber−packed needle extraction device, to-a consideration for the chemical structure of each fiber, should bebacco smoke and automobile exhaust were analyzed. The results

needed to reach the final conclusion, these results indicate that theclearly indicated a successful determination of EO from these com-adsorption behavior of VOCs was associated with the chemical

plex sample mixtures [19].

structure of the fabric, and that the proposed method could be applied to the development of a new evaluation method for preventing third−hand smoking pollution.

3. Particle−packed needle for typical VOCs in environmental

Smoker’s breath sample which collected at just after the final

samples
The particle−packed needle was developed as a miniaturized

puff was analyzed by GC−MS. The peaks of acetone, benzene andsample preparation device for the analysis of typical VOCs in envi-

toluene were also detected in non−smoker’s breath samples; how-ronmental air samples. For the sample preparation of the VOCs inever, these concentrations were clearly higher in the smoker’s

air samples, porous polymer beads or activated carbon (AC) parti-

breath. In addition, many VOCs were only detected in the smokers’

cles (150 to 180 µm diameter) were packed into the stainless steel

breath; especially 2,5−dimethyfurane has been recognized as a to-needle as shown in Fig. 1B. The extraction needles packed withbacco smoke biomarker in the smoker’s breath, and actually de-these particulate media allow a selection of suitable extraction me-

tected only in the smokers’ breath in this work. The time variations

dium for respective analytes. The target analytes are extracted onof the tobacco−related VOCs level in smoker’s breath are also

the sorbent when a gaseous sample is passed through the packed

measured, and it was confirmed that these VOCs were continu-

sorbent section in the needle. The extraction time for 50 mL gase-ously expired from the smoker’s breath for about 10 min, although

ous sample using the particle−packed needle was approximately 5

the concentrations of these VOCs were significantly higher overmin. The extracted analytes can then be thermally desorbed in thethe first 5 min. [23].

heated GC injector. The basic extraction/desorption and storage
3.2. Determination of fire accelerants−related VOCs for fire inves-performances of the particle−packed extraction needle for typicaltigation

VOCs were confirmed with an extraction sorbent consisted of a co-

Among the approximately 60,000 fires that occur in Japan every

polymer of methacrylic acid (MA) and ethylene glycol dimeth-year, arson represents the worst cause [24]. In the case of arson,

acrylate (EGDMA) [20].

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Ikuo Ueta

Fig. 4 Comparison of smoking−related VOCs adsorbed on 5 types of fabrics.
The concentration of ammonia was determined by a commercially available detection tube. Other compounds were determined by GC−MS in
the SIM mode. Modified from Fig. 3 in reference 23 with permission.
fire accelerants, such as gasoline and kerosene, are often used torepresentative fire accelerant VOCs were detected in Japanese cy-

start fires. Because these fire accelerants consist of mixtures ofpress up to weight losses of approximately 30%, and approxi-

VOCs, accurate and sensitive determinations of the VOCs found at

mately 50% in both pine and plywood samples.

the scenes of fires can be quite important in forensic investigations,

The proposed method was applied to the determination of fire

especially if arson is suspected from fire debris. In this work, a new

accelerants in simulated fires using two prefabricated rooms. The

method for fire investigations has been developed using a divinyl-

rooms used in these simulations were prefabricated rooms withbenzene (DVB)−packed extraction needle and subsequent GC

volumes of 15.1 m3, 2.7 m (width)×2.0 m (height)×2.8 m

analysis.

(depth), and were made to represent the typical interior of a small

The time−variation profiles of VOCs evaporated from fuel−Japanese room in winter. The first case was assumed to be a fire

spiked uncombusted samples of cotton fabric, carpet and wood,that resulted from misfueling of gasoline into a kerosene heater.

were measured for up to 48 h. The results indicated successful de-

The second case was assumed to be an arson fire in which approxi-

tection of these fuel−related compounds, as well as fingerprint pat-mately 4 L of kerosene was poured onto the floor before ignition.

terns. Fire accelerants−related VOCs, emitted from combusted car-

After the power of each fire had somewhat decreased from thepets and woods samples, were then measured. Although the sur-maximum, each fire was extinguished by water. Room air sample

faces of the carpet samples and the accelerants thereon were mostly

which suspected to be a headspace of the origin of the fire was ex-

combusted, the accelerants that had penetrated into the carpet sam-tracted using extraction needles 30 min after the extinction, and theples were successfully detected. For combusted woods samples, theextracted VOCs were analyzed in GC. Fig. 5 shows typical chro-―２
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CHROMATOGRAPHY, Vol.34 No.1 (2013)

matograms for separations of the air samples taken from the twothat obtained by the urine test strip, where only negative results

types of simulated fire scenes. The chromatogram shown in Fig.

were obtained for all these patients’ urine samples.

5A was monitored with an FID, and the chromatogram showed a

On the other hand, glycosylated hemoglobin level (HbA 1 c%)good agreement with that of headspace of pure gasoline. In Fig.

of the controlled diabetic patients was significantly higher than

5B, a set of characteristic aliphatic hydrocarbons clearly indicatedhealthy persons. Correlation between the HbA 1 c% level and thethe presence of kerosene at the fire scene. The above results also

breath acetone level of the diabetic patients was shown in Fig. 6.

suggest that the needle extraction method could be applied to not

Interestingly, a clear correlation was found between the HbA 1 c%

only the investigation of the arson−related fire, but also the investi-

and the concentration of the breath acetone.
The breath acetone concentration of a medically untreated type−gation of unintentional fire, such as misfueling [24].

2 diabetic patient was also determined. The HbA 1 c% in the last
several years was stable at the value of about 6.0%. The average

3.3. Human breath analysis
Acetone is normally included in human breath at ppb level, andbreath acetone concentration was range from 0.92 ppm to 1.20

has been regarded as a promising biomarker of diabetes. In thisppm, indicating a significant difference from a group of healthy

study, the MA/EGDMA particle−packed extraction needle was ap-

persons.

plied to the GC−MS analysis of breath acetone taken from 21 of

It is well−known that breath acetone level increases during fast-

controlled type−2 diabetes patients. All the patients have received

ing condition as the same physiology as insulin dependent diabetes.

either oral medication (O.M.) or insulin injection (I.I.) from the

Therefore, 4 healthy persons were fasted for 24 h, and breath ace-

doctor. The breath samples were collected in 1 L gas sampling bag

tone and urine acetone were monitored during this period. Typicalof Tedlar Bag, and its 50 mL was extracted by the particle−packed
needle. The breath acetone level in controlled diabetic patients wasin the range from 0.19 to 0.66 ppm, suggesting that no significant
difference was observed between healthy persons and controlled
type−2 diabetic patients. The results have a good agreement with

Fig. 5 Typical chromatograms for the separation of the air samples
containing fire accelerants−related VOCs obtained after simulated
fires.
(A) Simulation of misfueling of gasoline into kerosene heater and(B) simulation of an arson fire using kerosene. Conditions: gas
sampling volume, 100 mL ; column, HR−1 fused−silica capillarycolumn (30 m×0.25 mm I.D. film thickness 0.25 µm); oven temperature, 50oC (5 min) to 250oC (5 min) at 10oC /min ; monitoring
mode, (A) FID 250oC and (B) TIM (m/z : 50−250). (B) is modified
from Fig. 5 in reference 24 with permission.

Fig. 6 Relationships between the HbA 1 c% and breath acetone
concentration of controlled diabetic patients.
(A) Male patients and (B) female patients. Modified from Fig. 3 inreference 22 with permission.

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Ikuo Ueta

3.4. In−door room air analysis

profiles for the time variations of the breath and urine acetone under the fasting condition are illustrated in Fig. 7, where the X−axis

In recent years, much attention has been paid for the multiple

indicates the duration since last meal. Urine ketone level was meas-chemical sensitivity and/or sick building syndrome by VOCs in in-

ured by commercially available test strips. It can be seen that thedoor air. In Japan, the Ministry of Health, Labour and Welfare

acetone concentrations in the breath and urine were gradually in-(MHLW) adopted reference values and a measurement method forcreased after the fasting period of about 20 h, and then, rapidly de-

13 VOCs in indoor air [30]. Among them, two sample preparation

creased after the meal. A good correlation was found between themethods are proposed for typical VOCs: solvent desorption andacetone concentration of urine headspace and the results obtained

thermal desorption (TD) followed by GC analysis [31]. However,with urine ketone test strips. The correlation coefficient between

these methods have some disadvantages as described above. In ad-

the acetone concentration in the breath and urine samples in Fig. 7

dition, in the guideline established by the MHLW, the officially−

was 0.933, and similar higher correlations were also obtained fromstated sampling time of the gaseous sample is approximately 30

other three healthy subjects, r＝0.981, 0.980 and 0.918. Above re-min.

sults clearly demonstrated a good precision and versatility of pro-In this study, a novel needle−type sample preparation device was

posed method, and also suggested a future possibility as an initial

specially developed for the effective preconcentration of VOCs inscreening method for diabetes in medical scene [22].

indoor air samples. Four types of sorbent particles, including MA/
EGDMA, Tenax TA, DVB and AC−based particle of Shincarbon
ST, and their multi−bed combinations were investigated on the basis of the evaluation of their extraction and desorption performancefor standard samples. Successful extraction and desorption of
VOCs sample were accomplished using a double−bed sorbent
packed with DVB and AC particles in series. The optimum packing
length of the packed sections of DVB and AC were determined to
be 25 and 5 mm, respectively. This extraction needle was designed
for the extraction of low−volatility organic compounds (LVOCs)
on the DVB sorbent and high−volatility organic compounds(HVOCs) on the AC sorbent. To confirm this extraction behavior,
several VOCs were extracted by DVB−packed needle and DVB/
AC−packed needle as demonstrated in Fig. 8. For the DVB/AC−
packed extraction needle, the peak areas of all the investigated
VOCs increased linearly up to a sampling volume of approximately
800 mL (40 min), whereas for the DVB−packed needle, clear
symptoms of breakthrough were observed, especially for HVOCs.
After the optimization of several desorption conditions, such as
desorption temperature, desorption gas volume and desorption
time, more than 99.9% of extracted analytes were desorbed in asingle desorption without any observable carryover. Extraction recovery of the needle was also more than 99.9% for typical VOCs,
and the recovery was not susceptible to humidity when extracting
VOCs.
The LOQs of typical VOCs in the proposed method are less than
0.01 ng/L, showing the sufficient sensitivity of typical VOCs. The
relative standard deviations (RSDs) of the peak areas for each compound for 50 ng/L standard samples using one extraction needle (nFig. 7 Time variation profiles of breath and urine acetone inhealthy male under the fasting condition. Breath acetone (A) andurine acetone (B) were measured using the particle−packed extraction needle. Urine ketone level (C) was determined by commercially available test strips (Ketostix). Modified from Fig. 4 in reference 22 with permission.

＝5) were less than 5.0%, and the RSDs of needle−to−needle comparisons using five different extraction needles were less than
7.0%. The storage performance of the extracted VOCs in the extraction needle was also evaluated, and the results demonstrate an
excellent storage performance of the developed needle for up to 3

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CHROMATOGRAPHY, Vol.34 No.1 (2013)

Fig. 8 Sampling volume profiles of the DVB/AC−packed needle (circles) and DVB−packed needle (crosses). Conditions: standard gas sample
concentration, 50 ng/L; sampling rate, 20 mL/min. Modified from Fig. 5 in reference 25 with permission.
analytical method using the needle−type devices allows rapid, sim-days at room temperature.
The developed method was applied to the real indoor air analy-

ple and precise extraction/desorption for sensitive determination ofsis, and the results were compared to that obtained in the conven-

VOCs in GC, and also overcoming several drawbacks which aretional solvent extraction method. Four compounds, including tolu-

frequently found in traditional sample preparation methods. Further

ene, ethylbenzene, xylene and styrene, were quantified by both

applications of the needle extraction method could be expected foranalytical methods in 11 rooms. A significantly large data differ-other analysis, such as initial screening of several diseases based onence could be found especially at a high toluene concentration. One

the proposed breath analysis method and determination of VOCs inof the reasons for this difference could be the loss of volatile com-water and soil samples. In order to be a more popular analyticalpounds during solvent evaporation in the solvent extraction method

method, this technique should be further investigated, including de-[31]. At low concentrations, a good agreement was observed be-velopment of automatic extraction and desorption instruments withtween the data for these two extraction methods for all the analytes.

the needle−type extraction device.

Although further study is needed for a more precise comparison of
Acknowledgements

the developed extraction method and the conventional one, thebenefits of the needle extraction device, such as a simple and rapid

The author would like to express my sincere gratitude to Prof.

desorption process, for the analysis of indoor air VOCs were

Yoshihiro Saito (Toyohashi University of Technology) for his kindclearly demonstrated in the real sample analysis, and most of thesuggestion and valuable discussion. The author acknowledge Prof.

obtained results showed a good agreement with those of a conven-

Kiyokatsu Jinno and Prof. Yukio Hirata (Toyohashi University oftional solvent extraction method [25].

Technology) for their kind encouragement and advice. The author
also acknowledge the technical support of Dr. Hiroo Wada and Mr.
Koji Fujimura (Shinwa Chemical Industries, Ltd.), Mr. Yoshihisa

4. Conclusions
The needle−type extraction devices were successfully developed

Tsukahara (Hyogo Prefectural Emergency Management and Train-

for the analysis of VOCs in several environmental air samples. The

ing Center), Prof. Mitsuyoshi Okamoto (Meijo University), Dr.

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CHROMATOGRAPHY, Vol.34 No.1 (2013)

Ikuo Ueta

1201, 228−234.

Masahiko Hosoe (Ena Hospital), all medical staff in Ena Hospital,[17] Alonso, M.; Cerdan, L.; Godayol, A.; Anticó, E.; Sanchez, J.

Prof. Hiroyuki Sakamaki (Meijo University), Dr. Motoyuki

M. J. Chromatogr. A 2011, 1218, 8131−8139.

Ishiguro (Ishiguro Clinic), and Dr. Junpei Shindo (Environmental[18] Saito, Y.; Ueta, I.; Ogawa, M.; Jinno, K. Anal. Bioanal.

Technology Center Co., Ltd.). The author would express his grati-

Chem. 2006, 386, 725−732.

tude for support from Prof. Susumu Kawakubo (University of[19] Ueta, I.; Saito, Y.; Ghani, N. B. A.; Ogawa, M.; Yogo, K.;

Yamanashi) and Prof. Koji Otsuka (Kyoto University).

Abe, A.; Shirai, S.; Jinno, K. J. Chromatogr. A 2009, 1216,

Finally, the author gratefully thank the award committee and all2848−2853.

the members of the Japan Society for Chromatographic Sciences.

[20] Saito, Y.; Ueta, I.; Kotera, K.; Ogawa, M.; Wada, H.; Jinno,
K. J. Chromatogr. A 2006, 1106, 190−195.

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