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시료 희석 직접 주입 LC-MS/MS를 이용한 법화학 수용액 시료 중 카페인 신속 분석
최윤정,김희승,인문교,김진영,Choi, Yun Jeong,Kim, Hee Seung,In, Moon Kyo,Kim, Jin Young 대한약학회 2016 약학회지 Vol.60 No.3
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.
GC/MS를 이용한 소변 중 대마 대사체 분석의 측정불확도 평가
김진영,정재철,서승일,서용준,이정직,김종상,인문교,Kim, Jin-Young,Jeong, Jae-Chul,Suh, Sung-Ill,Suh, Yong-Jun,Lee, Jeong-Jik,Kim, Jong-Sang,In, Moon-Kyo 대한약학회 2008 약학회지 Vol.52 No.6
We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH), the major metabolite of ${\Delta}^9$-tetrahydrocannabinol, in urine sample by solid-phase extraction (SPE) and GC/MS detection. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day and inter-person validation were performed using statistical analysis of several indicative factors. Measurement uncertainty associated with target analyte in real forensic samples was estimated using quality control (QC) data. Traceability of measurement was established through traceable standards, calibrated volumetric glassware and volume measuring device. The major factors of contribution to combined standard uncertainty, were calibration linearity, inter-day repeatability and inter-person reproducibility, while those associated with preparation of analytical standards and sampling volume were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method was 12.05% for THCCOOH.
GC/MS를 이용한 모발 중 메스암페타민 및 암페타민 분석의 측정불확도 평가
김진영,김종상,김민경,이재일,서용준,인문교,Kim, Jin-Young,Kim, Jong-Sang,Kim, Min-Kyoung,Lee, Jae-Il,Suh, Yong-Jun,In, Moon-kyo 대한약학회 2007 약학회지 Vol.51 No.3
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%.