• 분석과학
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• 제21권2호
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• pp.93-101
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• 2008

SPME 분석기법은 헤드스페이스(Headspace: HS) 방식으로 기체상태의 흡착을 유도하거나, 액상시료에 직접 접촉하는 방식으로 분석대상 물질을 추출할 수 있다. 본 연구에서는 CAR/PDMS fiber를 이용하여, 액상시료의 VOC 분석을 시도하였다. 3 가지 변수 (흡착온도, 흡착시간, 교반여부)의 강약을 동시에 감안한 8가지 조합조건에서 분석효율을 조사하였다. (1) 용출온도: 30 대비 $50^{\circ}C$. (2) SPME fiber 시료노출시간: 10과 30 min. (3) 교반적용 여부: 무 교반 대비 1200 rpm. 8가지의 조합형 분석조건에서 HS-SPME 방식을 적용하여분석한 결과, S50-30 (stirring speed: 1200 rpm, exposure temp: 50oC, exposure time: 30 min)에서 가장 분석효율이 높게 나타났다. 가장 좋은 감도를 보인 S50-30방식의 분석 회수율을 GC에 직접주입하는 방식을 임의의 기준으로 평가하였을 때, 성분에 따라 상대 회수율이 45.5~68.5%로 나타났다. 본 연구의 결과, 3가지 변수 중에서 교반여부는 검량 특성을 결정짓는 가장 중요한 인자로 나타났다.

• Journal of Applied Biological Chemistry
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• 제49권4호
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• pp.180-185
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• 2006

Two different extraction procedures, SDE and SPME, were employed to determine a comprehensive and efficient fragrance profile of Korean Rosa hybrida. Both extraction methods could compensate for each other, covering compounds with diverse boiling point, polarities, and chemical properties. A total of 46 compounds were identified in Mi-hyang. The identified compounds were composed of 17 alcohols, 14 carbonyls, 7 aliphatic hydrocarbons, 2 terpene hydrocarbons, 4 benzenes, 1 ester, and 1 miscellaneous compound. Quantitatively, carbonyls($12.96{\sim}21.79%$ in essential oils of SDE and $2.89{\sim}8.44%$ in SPME headspace) and alcohols($7.98{\sim}11.73%$ in essential oils of SDE and $3.39{\sim}17.35%$ in SPME headspace) were dominant in Mi-hyang's volatiles.

• Mass Spectrometry Letters
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• 제8권1호
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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.

• 분석과학
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• 제13권4호
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• pp.412-422
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• 2000

실리콘 웨퍼 산업계의 청정실에서 사용되는 에어샤워기중 고분자로 제작된 부품들을 $100^{\circ}C$에서 30분간 다이나믹 해드 스페이스에서 가스로 용출한 후 GC-MS로 분석 하였다. 에어샤워기가 가동중인 청정실의 대기를 흡착관 튜브방식으로 채취하였고, 이러한 흡착관 튜브에 흡착된 유기화합물은 쏙시렛 용출법을 이용하여 용출한 후 GC-MS로 분석하였다. 에어샤워기의 제조 부품(electric over current relay, acryl plate. polycarbonate window, filter, fan housing, steel galvanized cold plate and canvas buffer)들로 부터의 분석결과 대부분의 성분들은 제조부품의 고분자 성분들에서 유래되었음을 확인 할 수 있었으며, 에어샤워기가 가동중인 청정실의 대기분석 결과와 비교 분석되었다. 이러한 분석결과의 비교 연구는 청정실내에서의 유기오염물질이 에어샤워기의 고분자 제조부품으로부터 유래 되었는지를 확인하게 해준다.

• 고려인삼학회:학술대회논문집
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• 고려인삼학회 2002년도 학술대회지
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• pp.238-252
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• 2002

In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

• 분석과학
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• 제14권5호
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• pp.392-399
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• 2001

생물시료에 존재하는 휘발성 유기화합물 중 n-butylbenzene과 1,2-dibromo-3-chloropropane (DBCP)를 기체크로마토그래피/질량분석기-선택이온검색법에 의해 수행하였다. 시료 중 휘발성 유기화합물은 $100{\mu}m$ polydimethyl siloxane (PDMS) fiber를 사용하여 headspace solid phase microextractio (SPME) 및 purge & trap 방법에 의해 추출 및 비교하였다. SPME에 의한 회수율은 n-butylbenzene의 경우 85.8%, DBCP의 경우 92.4%로 나타났고 검출한계는 각각 $0.15{\mu}g/kg$, $0.05{\mu}g/kg$로 나타났다. 반면, purge & trap의 경우 회수율은 n-butylbenzene의 경우 115.2%, DBCP의 경우는 80.9%로 나타났고 검출한계는 각각 $0.04{\mu}g/kg$ 및 $0.70{\mu}g/kg$로 나타나 두 방법에 있어 국내에서 규제하는 검출한계측면에서 큰 차이는 없었다.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3603-3609
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• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• 한국약용작물학회지
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• 제12권2호
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• pp.102-107
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• 2004

This study was carried out to establish an optimum method for identifying the volatile components of Magnolia ovobata Thunb. using the dynamic headspace (Purge & Trap) and simultaneous distillation and extraction (SDE) method. Between the two different identification analysis, the volatile components were more easily detected in the SDE than the Purge & Trap method. Among the identified volatile components, the 12 compounds were detected to have similar retention times and match quality within the 45 minutes in both identification methods. The maximum values of the major volatile components were detected differently by SDE and (Purge & Trap) method such as ${\alpha}-pinene$ (3.4, 18.2%), ${\beta}-pinene$ (3.5, 10.3%), l-limonene (5.2, 15.4%). These results indicated that the Dynamic Headspace (Purge & Trap) was much more reliable method for identifying the volatile components of Magnolia ovobata Thunb. as compared to the SDE method.

• 한국환경보건학회지
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• 제32권1호
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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.

• 한국연초학회지
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• 제35권1호
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• pp.7-12
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• 2013

A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.