• Title/Summary/Keyword: GC-SPME

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Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

  • Lee, In Ja;Ahn, Jae-Chan;Kim, Bogsoon;Chung, Deukmo
    • 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.

Analysis of Blood Toluene and Butane in Death Cases of Inhalant Abusers (사망사고 관련된 유해화학 물질 남용자들의 혈액 중 톨루엔과 부탄의 분석)

  • Kim, Nam-Yee;Yang, Young-Geun;Chung, Hee-Sun;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.577-582
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    • 1999
  • The blood toluene concentration was determined by using the GC/MSD with HS-SPME technique in postmortem blood, quantitatively. Butane gases was analyzed by using the GC/FID with HS technique in postmortem blood, qualitatively. Seventy five cases of dead associated with inhalation of glue or butane gases happened in Korea for the last 3 years (1996-1998). In 27 cases of deah due to glue sniffing, nine persons died as a result of a fall while intoxication and their blood tolucne concentration was fairly high in the range of $1.3{\sim}21.6{\mu}g/mL$. In case of death due to butane sniffing, fifty four persons died of acute butane gases inhalation or suffocation, and 6 persons died of butane gases as well as glue inhalation.

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Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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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.

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Determination of volatile compounds by headspace-solid phase microextraction - gas chromatography / mass spectrometry: Quality evaluation of Fuji apple

  • Lee, Yun-Yeol;Jeong, Moon-Cheol;Jang, Hae Won
    • Analytical Science and Technology
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    • v.30 no.2
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    • pp.68-74
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    • 2017
  • The volatile components in 'Fuji' apple were effectively determined by a headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 48 volatile components were identified and tentatively characterized based on National Institute of Standards and Technology (NIST) MS spectra library and the Kovats GC retention index I (RI). The harvested Fuji apples were divided into two groups: 1-methylcyclopropene (1-MCP) treated and non-treated (control) samples for finding important indicators between two groups. The major volatile components of both apples were 2-methylbutyl acetate, hexyl acetate, butyl 2-methylbutanoate, hexyl butanoate, hexyl 2-methylbutanoate, hexyl hexanoate and farnesene. No significant differences of these major compounds between 1-MCP treated and non-treated apples were observed during 1 month storage. Interestingly, the amount of off-flavors, including 1-butanol and butyl butanoate, in 1-MCP treated apples decreased over 5 months, and then increased after 7 months. However, non-treated apples did not show significant changes for off-flavors during 7 month storage (p<0.05). The non-treated apples also contained the higher levels of two off-flavors than 1-MCP treated apples. These two compounds, 1-butanol and butyl butanoate, can be used as quality indicators for the quality evaluation of Fuji apple.

Volatile Flavor Compounds in Commercial Milk by Static Headspace, Purge and Trap, Solid-Phase Microextraction (Static headspace, purge & trap 및 solid-phase microextraction을 이용한 시판우유의 휘발성 향기성분 분석)

  • Lee, Hong-Min;Lee, Ki-Woong;Chang, Chi-Hoon;Kim, Sung-Han
    • Korean Journal of Food Science and Technology
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    • v.38 no.6
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    • pp.738-741
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    • 2006
  • Volatile flavor compounds in commercial sterilized milk were analyzed and identified by static headspace, purge-and-trap, and solid-phase microextraction (SPME) methods. About 20 volatile compounds were identified by GC/MS, and aldehydes and ketones were the most distinctive and abundant compounds. Static headspace analysis allowed the identification of only the most abundant compounds, such as acetone. Five ketones (acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone), four aldehydes (2-methylbutanal, pentanal, hexanal, benzaldehyde) and dimethyl sulfide, all of which were responsible for off-flavor in milk, were found by the purge-and-trap and SPME methods. The two methods differed little in their release of these compounds, but they yielded different amounts in the extraction.

Essential Oil Analysis of Illicium anistum L. Extracts

  • Min, Hee-Jeong;Kim, Chan-Soo;Hyun, Hwa-Ja;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.6
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    • pp.682-688
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    • 2017
  • Fresh japanese anise (Illicium anisatum L.) tree leaves were collected and ground after drying. The essential oils of the leaves were analyzed by gas chromatography-mass spectrometry (GC-MS) using headspace (HS) and solid phase-microextra (SPME) methods. Volatile components of the leaves were identified 21 and 65 components in HS and SPME, respectively. The main components of the essential oils obtained by HS method were eucalyptol (36.7%), (+)-sabinene (15.61%), ${\delta}$-3-carene (6.87%), ${\alpha}$-pinene (6.07%), ${\gamma}$-terpinen (5.72%), ${\alpha}$-limonene (5.26%), ${\beta}$-myrcene (4.13%), ${\alpha}$-terpinene (4.04%) and ${\beta}$-pinene (3.73%). The other components were less than 3.5%. SPME method also showed that eucalyptol (17.88%) was main. The other were 5-allyl-1-methoxy-2 (13.29%), caryophyllene (6.09%), (+)-sabinene (5.60%), ${\alpha}$-ocimene (4.89%) and ${\beta}$-myrcene (3.73%), and the rest were less amounts than 3.5%. This work indicated that many more volatile components were isolated, comparing to the previous literature data and that SPME method was much more effective than HS method in the analysis of the volatile components.

Physiochemical Properties of Functional Oils Produced Using Red Yeast-Rice Ethanol Extracts and Diacylglycerol Oil (홍국쌀 에탄올 추출물과 Diacylglycerol Oil을 이용하여 제조한 기능성 유지의 이화학적 특성 연구)

  • Kim, Nam-Sook;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.2
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    • pp.201-208
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    • 2007
  • Functional oils (FOs) were produced from commercial diacylglycerol oil and red yeast rice extracts from 80% ethanol for 1 hr in a shaking water bath at $35^{\circ}C$ and 175 rpm. FOs contained (A) 600, (B) 1200, (C) 1800, and (D) 2280 ppm of red yeast-rice extracts, respectively. The Hunter a value and b value were risen whereas L value was reduced along with the increase of extract concentration. Content of monacolin K and total phenolic compounds in FOs significantly increased according to the increase of extract concentration. The oxidation stability of FOs was observed by Rancimat at $98^{\circ}C$. Induction time decreased according to the increase of extract concentration. The major volatile compounds of FOs were compared using the electronic nose (EN) system and solid phase microextraction (SPME) method combined with gas chromatograph/mass spectrometry (GC/MS). EN was composed of 12 different metal oxide sensors. Sensitivities (Rgas/Rair) of sensors from EN were analyzed by principal component analysis (PCA), whose proportion was 99.66%. For qualitative or quantitative analysis of volatile compounds by SPME-GC/MS, the divinylbenzene/carboxene/polydimethyl-siloxane fiber and sampling temperature of $50^{\circ}C$ were applied.

Analysis of Volatile Components of Sancho(Zanthoxylum schinifolium)by Solid Phase Micro Extraction (Solid Phase Micro Extraction을 이용한 산초의 휘발성 성분 분석)

  • 장희진
    • The Korean Journal of Food And Nutrition
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    • v.12 no.2
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    • pp.119-123
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    • 1999
  • Test of the optimum condition of solid phase micro extraction(SPME) was performed by use of 5 vol-atile components in dilute aqueous solution. Volatile components of Sancho(Zanthoxylum schinifolium) were isolated by SPME method and were analyzed by GC/MSD and compared with volatile compone-nts isolated by simultaneous distillation extraction (SDE) method. Total 31 components were identified by comparing gas chromatography retention time and mass spectral data. The major compounds were limonene geranyl acetate $\beta$-phellandrene phellandral mycene linalool rose oxide caproic acid and caprylic acid SPME sampling procedure was found to be a good method for qualitative analysis of the volatile components.

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Analysis of $C_4$-$C_{l2}$ Ozone precursors using SPME in ambient air (SPME를 이용한 대기중 $C_4$-$C_{l2}$ 오존전구물질 VOC분석)

  • 허귀석;유연미;이재환;이진홍
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2002.04a
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    • pp.217-218
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    • 2002
  • 대기환경 중의 오존은 유기용제의 사용 및 차량에서 배출되는 휘발성 방향족 화합물과 오존전구물질(ozone precursors)이 대기 중에서 광화학반응을 통하여 만들어지는 것으로 알려져 있다. 오존은 호흡기계통의 기관지염 및 감기, 현기증과 같은 인체의 건강상에도 매우 나쁜 영향을 초래하고 있어 이에 대한 모니터링이 중요한 과제로 대두되고 있다. 본 연구에서는 고가의 장비가 소요되는 기존의 분석법인 저온농축법과 흡착법을 이용하는 대신에 고체상 미량추출방법 (Solid-Phase Microextraction, 이하 SPME)을 이용하여 GC/MS로 대기 중 오존 VOC를 ppt 수준까지 빠르고 신속하게 분석하는 방법을 확립하였다. (중략)

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Analysis of Odorous compounds in Air by Solid Phase Microextraction (SPME) (SPME 분석법을 이용한 대기중 악취물질의 분석)

  • 허귀석;김대원
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2001.11a
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    • pp.340-341
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    • 2001
  • 대기중의 악취물질의 분석은 현행 우리나라 악취공정시험법에 고시되어 있으나 복잡한 농축장치를 필요로하고 조작법이 복잡하고 시간이 많이 소요된다. 주요 악취물질로서 암모니아, 메틸머캅탄, 황화수소, 이황화메틸, 아세트알데히드등은 극미량에서(pub) 악취를 발생시키는 악취 주요물질이다. 그러나 이 물질들은 흡착, 반응성이 커서 정확한 분석이 어렵다. 본 연구에서는 간단한 장치로서 시료농축이 가능하며, 간단히 GC injection에 주입, 분석할 수 있는 SPME법을 이용하여 악취물질을 신속하게 분석할 수 있는 분석법을 개발하고저 하였다. 분석방법에 대한 분석재현성, 분석한계를 조사하였으며, 이 분석방법이 앞으로 악취물질분석방법으로 활용될 수 있도록 기본 분석법을 확립하고자 하였다. (중략)

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