• Bulletin of the Korean Chemical Society
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• 제19권1호
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• pp.45-50
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• 1998

Most organophosphorus pesticides may be metabolized to yield some common phosphates in human or in animals, and these metabolites may be used as the exposure biomarkers to pesticides. In this study, we developed the extraction method of four phosphate metabolites from the spiked human urine in high recovery by the solid phase extraction with a reverse-phase cartridge (cyclohexyl silica) followed by the elution with methanol. The extracted urinary metabolites were derivatized with hexamethyldisilazane/trimethyl-chlorosilane/pyridine (2 : 1 : 10, v/v/v) and identified by gas chromatography/mass spectrometry. Calibration curve obtained from each metabolite standard using by GC/MS/SIM has shown good linearity and detection limits of metabolites were the range of 0.05-0.1 ㎍/㎖ in urine. Phenthoate, one of the organophosphorus pesticides, was orally administrated to rats. Four metabolites were detected in the rat urine. The results of this study may be applied to development of exposure biomarkers for monitoring of environmental pollutants.

• 분석과학
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• 제13권4호
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• pp.484-493
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• 2000

생물시료 중 존재하는 알킬페놀류, 클로로페놀류 및 비스페놀 A의 동시분석을 기체크로마토그래피-질량분석기-선택이온검색법에 의해 수행하였다. 시료 중 페놀류는 유기용매로 추출하고 정제과정은 Florisil과 silica 컬럼을 비교분석하였다. 회수율 실험은 각 생물시료에 1-ppm 정도를 첨가하여 수행하였다. 이들의 회수율은 83-116% 정도로 나타났고, 표준편차는 약 2.4-11.9%로 나타났다. 페놀류의 검출한계를 증진시키기 위하여, trimeaylsilyl(TMS) 유도체 방법을 도입하였다. 유도체화 시키지 않은 페놀과 TMS 유도체화된 페놀류의 기체크로마토그래피 성질을 연구하였다.

• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1693-1698
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• 2012

A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

• 한국미생물·생명공학회지
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• 제41권3호
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• pp.272-277
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• 2013

본 연구에서는 gas chromatography/mass spectrometry (GC/MS)와 gas chromatography (GC)를 이용하여 주목 식물세포 Taxus chinensis 유래 타르 성분을 최초로 동정/정량하였다. 또한 식물세포배양으로부터 항암물질 paclitaxel 정제를 위한 전처리 과정에서 이들 타르 성분들의 제거 양상을 확인하였다. GC/MS 분석을 통하여 체류시간을 비교한 결과, 5종류의 타르성분이 체류시간 6.374, 8.208, 15.209, 20.045, 24.474분에서 각각 2-picoline, o-xylene, 2,5-xylenol, 1-methylnaphthalene, acenaphthene이 동정되었다. 또한 표준물질을 이용한 spike testing을 수행한 결과 동일 물질임을 재확인 하였다. GC 분석을 통하여 동정된 5종류 타르성분을 정량한 결과, 메탄올 추출물에 총 0.6805 wt% (2-picoline: 0.2512 wt%, 2,5-xylenol: 0.1586 wt%, acenaphthene: 0.1240 wt%, 1-methylnaphthalene: 0.0942 wt%, o-xylene: 0.0525 wt%) 타르 성분이 존재하였다. 액-액 추출을 수행한 결과, 메탄올 추출물 시료 내 총 타르 성분의 양 대비 42%의 타르 성분이 제거됨을 확인할 수 있었다. 1-Methylnaphthalene, acenaphthene, 2,5-xylenol, 2-picoline의 경우에는 각각 75.90, 59.92, 35.94, 29.74%로 높은 제거율을 보인 반면 oxylene의 경우에는 10.86%의 제거율로 상대적으로 적게 제거됨을 알 수 있었다. 흡착제 처리 후 2-picoline과 o-xylene의 양도 상당히 줄었지만 이들 2 종류의 타르 성분을 제외한 나머지 세 종류의 타르 성분(2,5-xylenol, 1-methylnaphthalene, acenaphthene)은 완전히 제거됨을 확인할 수 있었다. 흡착제 처리 공정에서 제거되지 않은 두 종류의 타르 성분(2-picoline, o-xylene)은 헥산 침전 공정에 의해 완전히 제거 가능하였다.

• 대한화학회지
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• 제38권10호
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• pp.726-733
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• 1994

대기부유분진(air particulate material)중에 존재하는 다환방향족탄화수소(polycyclic aromatic hydrocarbons, PAH)를 신속하고 정확하게 분석하기 위하여 대기부유분진 시료를 10ml의 초임계유체($N_2O$ )로 30분간 추출 후 별도의 전처리와 농축과정 없이 GC/MS에서 분석하여 분석시간과 분석과정을 단축 및 단순화하였다. 시료로서 NBS 대기부유분진 인증표준기준물질(certified particulate reference material, CRM)1649와 서울의 도심에서 채취한 대기부유분진 시료를 이용하여 기존의 추출법 및 분석방법과 비교하였다. 그 결과 본 분석방법은 기존의 분석법에 비해 회수율은 상대적으로 작았으나 재현성이 좋았으며 분석과정이 간단하고 분석시간이 현저히 단축됨을 알 수 있었다.

• 생명과학회지
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• 제10권2호
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• pp.115-124
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• 2000

The present study was undertaken to separate the available components effectively, such as tetrodotoxin(TTX), docosahexaenoic acid(DHA, C22:6,ω-3) and eicosapentaenoic acid (EPA, C20:5,ω -3) from pufferfish liver waste, which are known to have high values as bioactive materials. By using ultrafiltration, it was possible to separate high contents of 68mg TTX from pufferfish liver waste. In contrast, by activated charcoal column, it was to obtain about 54mg TTX. The recovering ratios were 65.3% and 45.0% in the two different methods of ultrafiltration and activated charcoal column, respectively. From the results of HPLC and gas chromatography-mass spectrometry(GC-MS), the obtained toxins were identified to be TTX and its derivatives. In addition, it was also possible to obtain 72.3g DHA and 11.4g EPA from 1kg of pufferfish liver by high performance liquid chromatography (HPLC). These amounts of DHA and EPA were also 17.70% and 1.04% in the total lipid of pufferfish liver oil from analysis of gas chromatography(GC), respectively.

• Bulletin of the Korean Chemical Society
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• 제30권7호
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• pp.1489-1496
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• 2009

This study was done for the determination and excretion profile of adrenosterone and its metabolites in human urine using both liquid chromatography with atmospheric pressure chemical ionization mass spectrometry and gas chromatography with mass spectrometry. Adrenosterone and its two metabolites were detected in human urine after administration a healthy volunteer with 75 mg of adrenosterone. We found that adrenosterone-M1 ($C_{19}H_{26}O_3$) was a reduction and adrenosterone-M2 ($C_{19}H_{26}O_4$) was a hydroxylation at C-ring, which did not know the exact position of the C-ring. The adrenosterone parent was detected by GC/TOF-MS, but not detected by LC/APCI/MS because of low intensity. Adrenosterone and its two metabolites were excreted as their glucuronided fractions. The recovery of this method ranged from 100.7 to 118.4% and the reproducibility and accuracy test were 85.5 to 112.0% and 1.1 to 8.4%, respectively. The excretion studies showed that adrenosterone and its metabolites were detectable in human urine during a 48 h period after oral administration, with maximum level of excretion at 4.1 h. The glucuro-/sulfaconjugated ratio of adrenosterone, M1 and M2 was 0.73 ${\pm}$ 0.03, 0.96 ${\pm}$ 0.06 and 0.89 ${\pm}$ 0.03 (n = 6), respectively. The amounts of adrenosterone excreted in urine were 14.75 ng for 48 h. Also, the maximum level of androsterone and 11$\beta$-hydroxy androsterone, which were endogenous steroids, were reached 4.1 h after the oral administration of adrenosterone.

• Bulletin of the Korean Chemical Society
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• 제32권5호
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• pp.1547-1553
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• 2011

An effective analytical method of gas chromatography/mass spectrometry (GC/MS) was developed for the rapid determination of essential oils in the crude extract of Acorus species (Acorus gramineus, Acorus tatarinowii, and Acorus calamus). Major phenypropanoids (${\beta}$,${\alpha}$-asarone isomers, euasarone, and methyleugenol) and ${\beta}$-caryophyllene in Acorus species were used as marker compounds and determined for the quality control of herbal medicines. To extract marker compounds, various extraction techniques such as solvent immersion, mechanical shaking, and sonication were compared, and the greatest efficiency was observed with sonication extraction using petroleum ether. The dynamic range of the GC/MS method depended on the specific analyte; acceptable quantification was obtained between 10 and 2000 ${\mu}g/mL$ for ${\beta}$-asarone, 10 and 500 ${\mu}g/mL$ for ${\alpha}$-asarone, 10 and 200 ${\mu}g/mL$ for methyleugenol, and between 5 and 100 ${\mu}g/mL$ for ${\beta}$-caryophyllene. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision, with a relative standard deviation < 10%. Overall limits of detection were approximately 0.34-0.83 ${\mu}g/mL$, with a standard deviation (${\sigma}$)-to-calibration slope (s) ratio (${\sigma}$/s) of 3. The limit of quantitation in our experiments was approximately 1.13-3.20 ${\mu}g/mL$ at a ${\sigma}$/s of 10. On the basement of method validation, 20 samples of Acorus species collected from markets in Korea were monitored for the quality control. In addition, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were performed on the analytical data of 20 different Acorus species samples in order to classify samples that were collected from different regions.

• Archives of Pharmacal Research
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• 제28권9호
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• pp.1086-1091
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• 2005

An analytical method was developed for evaluating the cannabidiol (CBO), cannabinol (CBN), ${\Delta}^9-tetrahydrocannabinol$ $({\Delta}^9-THC)$ level in human hair using gas chromatography-mass spectrometry (GC-MS). Hair samples (50mg) were washed with isopropyl alcohol and cut into small fragments (< 1mm). After adding a deuterated internal standard, the hair samples were incubated in 1.0M NaOH for 10 min at $95^{\circ}C$. The analytes from the resulting hydrolyzed samples were extracted using a mixture of n-hexane-ethyl acetate (75:25, v/v). The extracts were then evaporated, derivatized, and injected into the GC-MS. The recovery ranges of CBD, CBN, and ${\Delta}^9-THC$ at three concentration levels were $37.9-94.5\%$ with good correlation coefficients $(r^2>0.9989)$. The intra-day precision and accuracy ranged from $-9.4\%\;to\;17.7\%$, and the inter-day precision and accuracy ranged from $-15.5\%\;to\;14.5\%$, respectively. The limits of detection (LOD) for CBD, CBN, and ${\Delta}^9-THC$ were 0.005, 0.002, and 0.006 ng/mg, respectively. The applicability of this method of analyzing the hair samples from cannabis abusers was demonstrated.

• Journal of Ginseng Research
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• 제42권1호
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• pp.57-67
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• 2018

Background: Ginseng contains many small metabolites such as amino acids, fatty acids, carbohydrates, and ginsenosides. However, little is known about the relationships between microorganisms and metabolites during the entire ginseng fermentation process. We investigated metabolic changes during ginseng fermentation according to the inoculation of food-compatible microorganisms. Methods: Gas chromatography mass spectrometry (GC-MS) datasets coupled with the multivariate statistical method for the purpose of latent-information extraction and sample classification were used for the evaluation of ginseng fermentation. Four different starter cultures (Saccharomyces bayanus, Bacillus subtilis, Lactobacillus plantarum, and Leuconostoc mesenteroide) were used for the ginseng extract fermentation. Results: The principal component analysis score plot and heat map showed a clear separation between ginseng extracts fermented with S. bayanus and other strains. The highest levels of fructose, maltose, and galactose in the ginseng extracts were found in ginseng extracts fermented with B. subtilis. The levels of succinic acid and malic acid in the ginseng extract fermented with S. bayanus as well as the levels of lactic acid, malonic acid, and hydroxypruvic acid in the ginseng extract fermented with lactic acid bacteria (L. plantarum and L. mesenteroide) were the highest. In the results of taste features analysis using an electronic tongue, the ginseng extracts fermented with lactic acid bacteria were significantly distinguished from other groups by a high index of sour taste probably due to high lactic acid contents. Conclusion: These results suggest that a metabolomics approach based on GC-MS can be a useful tool to understand ginseng fermentation and evaluate the fermentative characteristics of starter cultures.