• 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.

• 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.

• 한국식품과학회지
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• 제19권3호
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• pp.279-284
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• 1987

우리나라의 야생산채류중 물쑥과 파드득나물의 휘발성 성분을 수증기 증류법으로 추출해서 GC와 GC-MS조합에 의하여 분석하였다. 물쑥에서는 ${\alpha}-pinene$, camphene, ${\beta}-pinene$, myrcene, limonene, ${\alpha}-terpinene$ 및 caryophllene의 7가지 성분이, 파드득나물에서는${\alpha}-pinene$과 ${\beta}-pinene$의 두가지 성분이 확인되었다. 파드득나물의 나머지 성분은 elemene, caryophyllene 및 humulene으로 추정된다.

• Applied Biological Chemistry
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• 제31권4호
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• pp.394-399
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• 1988

야생 식용 산채류중 씀바귀와 비름의 휘발성 풍미성분을 수증기 증류법으로 추출해서 GC와 GC-MS 조합에 의하여 분석하였다. 씀바귀에서는 alcohols류 13종, esters류 9종, aldehydes류 12종, ketones류 6종, hydrocarbons류 9종, acids류 6종, phenols류 3종 그리고 기타 3종의 총 61 성분이 확인 되었다. 비름에서는 alcohols류 15종, esters류 5종, aldehydes류 13종, ketones류 8종, hydrocarbons류 3종, acids류 7종, 기타 5종의 총 56 성분이 확인되었다.

• 한국식품과학회지
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• 제25권5호
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• pp.494-501
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• 1993

The volatile flavor components of traditional and commercial kochujang were collected by simultaneous steam distillation-extraction (SDE) method. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC/MS). Tested kochujang included Sunchang kochujang prepared with glutinous rice, Boeun kochujang prepared with barley, Sachun kochujang prepared with wheat and commercial kochujang. One hundred and twelve volatile flavor components which included 30 esters, 15 alcohols, 14 aldehydes, 13 acids, 9 ketones, 7 alkenes, 6 phenols, 3 alkanes, 3 pyrazines, 2 benzenes and 2 furans were identified. The major volatile compounds in traditional and commercial kochujang were 2-methyl propanal and ethanol, which represented $21{\sim}36%\;and\;2{\sim}44%$ of total GC peak area, respectively.

• 한국식생활문화학회지
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• 제3권2호
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• pp.207-210
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• 1988

한국산(韓國産) 야생 산채류인 맑은대쑥의 휘발성 풍미성분을 수증기 증류법으로 추출해서 GC와 GC-MS 조합에 의하여 분석하였다. 본 연구에서 hydrocarbons 17종류, alcohols 6종류, aldehydes 2종류, oxide 1종류, 그리고 furans 3종류 등 총 29개의 성분이 확인되었다.

• 분석과학
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• 제34권2호
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• pp.68-77
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• 2021

Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

• Preventive Nutrition and Food Science
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• 제16권1호
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• pp.45-54
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• 2011

Volatile components in commercial pine needle (Pinus densiflora S. and Z.) powder were extracted using simultaneous steam distillation and a solvent extraction (SDE) apparatus, and were analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 230 compounds divided into 13 groups were identified, which included alcohols (42), ketones (39), aldehydes (32), terpenes (30), alkenes (17), esters (14), furans (14), benzenes (10), alkanes (8), napthalenes (7), acids (6), miscellaneous compounds (6), and phenols (5). Among the 230 compounds identified, 96 compounds were positively confirmed and quantified, and the rest of the compounds were tentatively identified. The major volatile components identified at relatively high levels were dodecanoic acid, hexadecanoic acid, hexanal, benzaldehyde, (Z)-3-hexen-1-ol, 1-penten-3-one, limonene, and $\beta$-caryophyllene oxide. Among the groups, terpenes accounted for 60.18% of the total concentration of all the volatile components. Some volatile components might account for the unique aroma and the biological activity of the sample.