• 분석과학
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• 제15권3호
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• pp.221-228
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• 2002

MX [3-chloro-4(dichloromethyl)-5-hydroxy-2(5H)-furanone]는 수돗물의 소독을 위해 첨가한 염소와 수중의 유기물이 반응하여 생성되는 강력한 변이원성 물질이다. 본 논문에서는 GC/MS를 이용하여 유도체화 시약인 2% 황산-methanol, iso-propanol, sec-butanol, n-butanol을 이용하여 MX의 유도체화를 비교하였으며, 이온화 방법으로 EI 와 NCI를 비교한 결과, NCI 방법에서 검출 한계가 1.25 pg으로 EI 방법에서는 25 pg이였으며, 25~2500 pg 범위에서 직선성을 나타내었다.

• Biotechnology and Bioprocess Engineering:BBE
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• 제11권1호
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• pp.38-42
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• 2006

When whole cells are subjected to pyrolysis gas chromatography/mass spectrometry (Py-GC/MS) analysis, it provides biochemical profiles containing overlapping signals of the majority of compounds. To determine marker compounds that discriminate embryogenic calluses from nonembryogenic calluses, samples of embryogenic and nonembryogenic calluses of five higher plant species were subjected to Py-GC/MS. Genetic programming of Py-GC/MS data was able to discriminate embryogenic calluses from nonembryogenic calluses. The content ratio of 5-meyhyl-2-furancarboxaldehyde and 5-(hydroxymethyl)-2-furancarboxaldehyde was greater in nonembryogenic calluses than in embryogenic calluses. However, the content ratio of phenol, p-cresol, and $^1H-indole$ in embryogenic calluses was 1.2 to 2.4 times greater than the ratio in nonembryogenic calluses. These pyrolysates seem to be derived from the components of the cell walls, which suggests that differences in cell wall components or changes in the architecture of the cell wall playa crucial role in determining the embryogenic competence of calluses.

• 약학회지
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• 제47권3호
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• pp.142-147
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• 2003

Gas chromatography-mass spectrometric (GC-MS) procedure is presented for the simultaneous qualification and quantitation of methamphetamine (MA), amphetamine (AMP), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxyethylamphetamine (MDEA) in human hair. The method procedure involves decontamination of hair with distilled water and acetone, acidic hydrolysis, extraction in the presence of deuterated internal standards, and GC-MS analysis after derivatization with trifluoroacetic anhydride (TFAA) in ethylacetate. The limit of detection for 5 drugs were about 0.1∼0.15 ng/mg using 30 mg hair sample. Coefficient variations of correlation ranged from 0.9941 to 0.9993. The recoveries of these drugs were found to be 93.4∼104.4％. The concentrations of AMP, MA, MDA, and MDMA in abusers' hair samples were measured 0.17∼2.88, 2.09∼18.34, 0.24∼3.83, and 3.10∼22.81 ng/mg, respectively. The ratios of MA/AMP and MDMA/MDA ranged 5.67∼49.57 and 4.78∼54.31, respectively. This assay has been successfully utilized in the evaluation of the deposition of amphetamine-type stimulants (ATS) in human hair.

• Bulletin of the Korean Chemical Society
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• 제30권10호
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• pp.2287-2293
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• 2009

Gas Chromatography-Mass Spectrometry (GC-MS) fingerprint analysis, Principle Components Analysis (PCA), and Hierarchical Cluster Analysis (HCA) were introduced for quality assessment of Curcuma longa L. (C. longa). The GC-MS fingerprint method was developed and validated by analyzing 33 batches of samples of C. longa from different geographic locations. 18 chromatographic peaks were selected as characteristic peaks and their relative peak areas (RPA) were calculated for quantitative expression. Two principal components (PCs) were extracted by PCA. C. longa collected from Guizhou and Fujian were separated from other samples by PC1, capturing 71.83% of variance. While, PC2 contributed for their further separation, capturing 11.13% of variance. HCA confirmed the result of PCA analysis. Therefore, GC-MS fingerprint study with chemometric techniques provides a very flexible and reliable method for quality assessment of C. longa.

• 약학회지
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• 제51권3호
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• pp.206-213
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• 2007

Recently estimating the uncertainty of an analytical result has become an essential part of quantitative analysis. This study describes the uncertainty of the measurement for the determination of methamphetamine and its major metabolite amphetamine in human hair, The method consists of washing, drying, weighing, incubation and extraction with methanolic HCI solution, clean-up, trifluoroacetyl derivatization, and qualification/quantification of residues by gas chromatography/mass spectrometry (GC/MS). Traceability of measurement was established through traceable standards and calibrated volumetric equipment and measuring instruments. Measurement uncertainty associated with each analyte in real samples was estimated using quality control (QC) data. The main source of combined standard uncertainty comprised two components, which are uncertainties associated with calibration linearity and variations in QC, while those associated with preparation of analytical standards and sample weighing were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method ranged for individual analytes from 4.99 to5.03%.

• 분석과학
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• 제14권6호
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• pp.471-475
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• 2001

$85{\mu}m$-polyacrylate(PA) 와 $100{\mu}m$-polydimethylsiloxane(PDMS) fiber를 사용하여 물증의 DBCP와 n-butylbenzene을 추출한 후 GC-MS로 분석하는 방법을 연구하였다. SPME 과정에 영향을 미치는 인자들, 즉 추출 시간, 주입 길이, 주입 온도, 탈착 시간 및 탈착 온도들에 대한 최적화 조건을 조사하였다. 검량선의 직선성(correlation coefficient, R)은 0.99 이상이었으며, 본 분석법의 검출한계는 1.5 와 $10.8{\mu}g/L$ 이었고, 분석법의 재현성은 RSD 10.4와 14.4 % 였다.

• 분석과학
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• 제7권4호
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• pp.441-453
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• 1994

수질에서 유해물질을 농축하는 방법으로 액체 추출법과 고체상 추출법을 GC/MS를 검출기로 사용하여 비교하였다. 비휘발성 유해물질 중 11종의 산과 44종의 염기/중성 화합물들을 reagent water에 첨가하여 분석한 결과, 액체추출법은 54종의 화합물에 대해 91%의 평균회수율과 4.6%의 평균상대표준편차를 나타내었으며, 고체상 추출법은 52종의 화합물에 대해 63%의 평균회수율과 8.9%의 평균상대표준편차를 보였다. 두 방법의 검출한계는 $1{\sim}5{\mu}g/l$였다.

• Archives of Pharmacal Research
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• 제26권9호
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• pp.697-705
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• 2003

The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

• 분석과학
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• 제32권3호
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• pp.88-95
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• 2019

This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

• Journal of Applied Biological Chemistry
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• 제66권
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• pp.144-152
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• 2023

Two different extraction methods were used to evaluate the medical value of common rue, Ruta graveolens L. (RGL). The results of our 2,2-diphenyl-1-picrylhydrazyl and 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid assays indicated that the antioxidant activity of RGL essential oil extract obtained through steam distillation was very low, whereas ethanol (EtOH) extracts of RGL showed higher antioxidant activity. RGL essential oil was extracted by steam distillation and characterized by GC/MS analysis. Furthermore, EtOH extracts of RGL were obtained under reflux and analyzed by HPLC/PDA. The GC/MS results indicated that the ketone compounds 2-undecanol acetate, nonyl cyclopropanecarboxylate, and 2-nonanone accounted for more than 70% of the composition of RGL essential oil. The HPLC/PDA analyses indicated that the RGL extracts were rich in phenolic compounds such as protocatechuic acid, rutin, psoralen, xanthotoxin, and bergapten, among which rutin was the most abundant. Collectively, our results demonstrated that RGL contains high levels of phenolic compounds and could thus be commercialized as a valuable plant-derived antioxidant.