• Journal of Environmental Health Sciences
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• v.32 no.1 s.88
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• pp.67-70
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• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

• Analytical Science and Technology
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• v.26 no.5
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• pp.326-332
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• 2013

Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

• Analytical Science and Technology
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• v.16 no.6
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• pp.458-465
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• 2003

The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

• Analytical Science and Technology
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• v.20 no.5
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• pp.361-369
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• 2007

Uncomfortable odor emitted from air conditioning system is the main cause of indoor air quality deterioration. To solve evaporator odor problems, odor active compounds, have to be identified then the quality of the product can be improved its quality. Because evaporator odor in exhaust gas has low odor intensity and discontinuity, it is very difficult to collect and analyze sample. In this study through the identification of odor compounds in condensed water, the evaluation of the eraporator was tested. Odor compounds were extracted from water by headspace-solid-phase microextraction (HS-SPME) method. The single odor was separated by GC/FID/Olfactometry (GC/FID/O) and odor active compounds were identified by GC/AED and GC/MS. Compared to air sample, result of sensory evaluation and the single odor compound appeared similarly. It was identified that odor active compounds have functional group containing oxygen such as alcohols and acids. Evaluation method of odor active compounds using condensed water in evaporator appeared effective on the side of simplicity of collection, low expanse and rapid analysis.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.44 no.2
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• pp.154-158
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• 1999

Volatile flavor compounds from perilla leaves were extracted and analyzed with different methods, head-space analysis (HS), simultaneous steam distillation and extraction (SDE) , and solvent extraction (SE), and to compare their efficiencies for quick analysis. Over 30 volatile compounds were isolated and 28 compounds were identified by GC/MSD. Major compound was perillaketone showing the compositions of which were 92% in SDE method, 86% in headspace analysis, and 62% in solvent extraction method. For quick evaluation of leaf flavor in perilla, it was desirable because the headspace analysis method had a shorter analyzing time and smaller sample amount than the other methods.

• Korean Journal of Food Science and Technology
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• v.37 no.5
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• pp.695-701
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• 2005

Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

• Analytical Science and Technology
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• v.20 no.3
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• pp.237-245
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• 2007

The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

• Analytical Science and Technology
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• v.14 no.5
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• pp.392-399
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• 2001

The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

• Bulletin of the Korean Chemical Society
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• v.30 no.11
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• pp.2675-2679
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• 2009

This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

• Mass Spectrometry Letters
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• v.8 no.1
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• pp.18-22
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• 2017

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.