• 약학회지
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• 제33권3호
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• pp.156-160
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• 1989

A gas-chromatographic determination method of thiamin which use a quantitative cleavage of thiamin to 4-methyl-5-(2-hydroxyethyl)thiazol [I] and solvent extraction of the analyte prior to GC injection was modified. A column chromatographic procedure using a reversed phase, high capacity solid phase cartridge was applied to the clean-up of the analyte. Thiazol derivative[I] was quantitatively recovered upon the column method. Acetanilide, an internal standard, has a good recovery through the analytical procedure. The method has analytical precision of 2% or less in the coefficient of variation.

• 한국환경과학회지
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• 제18권12호
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• pp.1369-1381
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• 2009

The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

• 약학회지
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• 제44권5호
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• pp.384-390
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• 2000

Metabolism study of the dye, benzidine, was performed by gas chromatography-mass selective detector (GC/MSD) in the urine of rats orally administered 100 mg/kg benzidine. Urine samples were collected in metabolic cages for 0-24, 24-48, and 48-72 hrs. Ten ml of the urine was extracted with XAD-2 resin and the XAD-2 column was eluted with methanol. After evaporation, benzidine and its metabolites were extracted with diethyl ether (for non-conjugated fraction). For conjugated metabolites, $\beta$-glucu-ronidase was added to the aqueous layer that was incubated for 1 hr at 5$0^{\circ}C$ and the aqueous layer was extracted as in non-conjugated fraction. Aliquot of trimethylsilylated derivatives was applied to the GC/MSD. The mutagenicity of benzidine and its acetylated metabolites was tested by histidine/reversion assay. Five metabolites observed and confirmed either by electron impact and chemical ionization modes of the GC/MSD, or authentic compounds were monoacetyl-, diacetyl-, hydroxyacetyl-, hydroxydiacetyl-, and hydroxy-benzidine. Monoacetyl-benzidine was more potent than benzidine in histidine/reversion assay. This data indicates that monoacetylation of benzidine may be one of the metabolites produced in metabolic activation process.

• Journal of Nutrition and Health
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• 제16권2호
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• pp.107-114
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• 1983

There has been no specific test available for identifying the sesame oil among common edible oils. As the contents of sesamin and the ratio of sterols allowed the estimation for the genuine sesame oil, the author investigated to establish some instrumental methods for verification of genuine sesame oil and its distribution in the market. The sesame oil was saponified and the sesamin and sterols were isolated from the unsaponiable fraction by Florisil column chromatography. The individual components were determined by gas- chromatography and sesamin standard (purified sesamin) was obtained by silicagel column chromatography. The gas- chromatographic condition using Flame Ionization Detector supported on 10% OV-101 with di-(2-ethylhexyl) sebacate as an internal standard was suitable, and quantitation of sesamin and sterols, including campesterol, stigmasterol and ${\beta}-sitosterol$ was carried out. The results of this study showed that contents of sesamin in genuine sesame oil were 0.3-0.5% and the ratio of stigmasterol to compesterol was 0.3-0.6 and ${\beta}-sitosterol$ to campesterol 3.0-3.8. The 50 samples from the markets in Seoul were composed of 70% genuine sesame oil, and others were mixed with palm oil, rape seed oil and soybean oil.

• 분석과학
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• 제31권3호
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• pp.112-121
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• 2018

The hydrothermal carbonization method has received great attention because of the conversion process from biomass. The reaction produces various products in hydrochar, bio-liquid, and gas. Even though its yield cannot be ignored in amount, it is difficult to find research papers on bio-liquid generated from the hydrothermal carbonization reaction of biomass. In particular, the heterogeneity of feedstock composition may make the characterization of bio-liquid different and difficult. In this study, bio-liquid from the hydrothermal carbonization reaction of food wastes at $230^{\circ}C$ for 4 h was investigated. Among various products, fatty acid methyl esters were analyzed using two different extraction methods: liquid-liquid extraction and column chromatography. Different elutions with various solvents enabled us to categorize the various components. The eluents and fractions obtained from two different extraction methods were analyzed by gas chromatography with a mass spectrometer (GC/MS). The composition of the bio-liquid in each fraction was characterized, and seven fatty acid methyl esters were identified using the library installed in GC/MS device.

• 한국응용곤충학회지
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• 제16권4호
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• pp.221-227
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• 1977

Polychlorinated Biphenyls (PCBs)는 유기염소계 농약잔류성분의 GLC분석에 간섭하는 물질이다. 본 실험에서는 PCBs의 존재하에 대표적인 유기염소계 농약 및 이들의 주요대사물의 분석을 목저르오 Florisil column상에서 PCBs와 농약성분의 분리를 시도하였다. 활성화한 Florisil column에서 $\alpha-BHC,\; \gamma-BHC$, Heptachlor, epoxide, Dielerin, p.p'-DDD, p.p'-DDT와 Aroclor 1254는 완전히 그리고 정량적으로 분리하여 GLC로 분석할 수 있었다. Heptachlor와 Aldrin은 Aroclor와 함께 elution되나 Chromatogram 상에서 정량이 가능하였다. 본 시험에서 사용한 Florisil column chromatography는 많은 시료를 대상으로 한 잔류농약의 효과적 분석에 사용될 수 있다.

• 대한화학회지
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• 제31권5호
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• pp.425-433
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• 1987

모세관 컬럼을 사용한 기체크로마토그래피로 19종 유기염소제 농약의 분리를 검토하였고, 쌀에 첨가한 농약들의 회수율을 구하여 봄으로써 실제분석에 대한 본 방법의 응용 가능성을 조사하였다. SE-30과 OV-17모세관 컬럼의 분리를 비교하여 본 결과 OV-17 컬럼(25m ${\times}$ 0.20mm, 0.27${\mu}$m 두께)으로 분리가 잘되고 있으며, splitless방식으로 주입한 농약들의 머무른 시간과 봉우리 면적에 대한 상대표준 편차가 최대로 0.16%와 8.2%이었다. 쌀에 첨가된 농약의 회수율은 대부분 85%이상이었고 분석 결과에 대한 상대표준편차가 가장 큰 것이 11.4%로서 흔적량의 잔류농약분석에서 비교적 정밀도가 좋음을 확인하였다.

• 대한화학회지
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• 제29권5호
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• pp.503-509
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• 1985

농산물에 잔류되어 있는 16종의 유기염소제 농약들을 추출하여 cleanup한 것을 기체 액체 크로마토그래피법으로 분리, 정량하였다. 5% QF-1 정지상의 분리관을 주로 사용하였으며 3% OV-17관과 DC-200/2.5% QF-1 혼합관을 보조적으로 사용하였다. $^{63}Ni$ electron capture detector를 사용하여 각 농약 성분을 검출하였다. 대부분의 농약에 대한 감응곡선은 직선성을 나타냈고 일부는 약간 휘었으나 정량에는 별 지장을 주지 않았다. 16종의 농약을 13종의 농산물에 가하여 분석한 결과 대부분은 85% 이상의 평균회수율을 보였으며 각 5회 분석결과에 대한 상대평균편차는 12.1% 이하로서 AOAC에서 정한 기준을 만족하였다.

• 생약학회지
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• 제23권1호
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• pp.29-33
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• 1992

The essential oils of Lycopus lucidus have been studied. The essential oil obtained from the dried herba by steam distillation followed by fractionation by column chromatography was analysed by gas chromatography-mass spectrometry(GC-MS). The compounds identified by GC-MS were carvacrol, 2,5-dimethoxy-p-cymene, trans-caryophyllene, spathurenol and $trans-{\beta}-farnesene$. Two compounds, thymol and caryophyllene were isolated by silica gel column chromatography and analyzed by TLC, IR, Mass and NMR. And the weak diuretic effects of essential oil and water extract from the dried drugs were observed in rats.

• KSBB Journal
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• 제30권4호
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• pp.141-147
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• 2015

The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.