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使用快速气相色谱-质谱法快速定量尿液中11-去甲-δ9-四氢大麻酚-9-羧酸

Rapid quantification of urinary 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid using fast gas chromatography-mass spectrometry.

作者信息

Jamerson Matthew H, Welton Robert M, Morris-Kukoski Cynthia L, Klette Kevin L

机构信息

Navy Drug Screening Laboratory, 320 B Street, Great Lakes, Illinois 60088-2815, USA.

出版信息

J Anal Toxicol. 2005 Oct;29(7):664-8. doi: 10.1093/jat/29.7.664.

Abstract

Human urine specimens that were determined to be presumptively positive for metabolites of delta9-tetrahydrocannabinol by immunoassay screening were assayed using a novel fast gas chromatography-mass spectrometry (FGC-MS) analytical method to determine whether this method would improve the efficiency of specimen processing without diminishing the reliability of metabolite identification and quantification. Urine specimens were spiked with deuterated internal standard, subjected to solid-phase extraction, and derivatized using tetramethylammonium hydroxide and iodomethane. The methyl ester/methyl ether derivatives were identified and quantified using both a traditional GC-MS method and the newly developed FGC-MS method. The FGC-MS method was demonstrated to be linear between 3.8 and 1500 ng/mL 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (11-nor-delta-THC-COOH). The intrarun precision of 15 replicates of a 15 ng/mL control and the interrun precision of 161 sets of 7, 15, and 60 ng/mL controls were acceptable (coefficients of variation < 5.5%). The FGC-MS method was demonstrated to be specific for identifying 11-nor-delta9-THC-COOH and none of 43 tested substances interfered with identification and quantification of 11-nor-delta9-THC-COOH. Excellent data concordance (R2 > 0.993) was found for two specimen sets assayed using both methods. The FGC-MS method, when compared with a traditional GC-MS method, reduces total assay time by approximately 40% with no decrease in data quality.

摘要

通过免疫分析筛选确定为9-四氢大麻酚代谢物推定阳性的人类尿液标本,采用一种新型快速气相色谱-质谱联用(FGC-MS)分析方法进行检测,以确定该方法是否能在不降低代谢物鉴定和定量可靠性的情况下提高标本处理效率。尿液标本加入氘代内标,进行固相萃取,并用氢氧化四甲铵和碘甲烷衍生化。使用传统的气相色谱-质谱联用方法和新开发的FGC-MS方法对甲酯/甲醚衍生物进行鉴定和定量。FGC-MS方法在3.8至1500 ng/mL的11-去甲-9-四氢大麻酚-9-羧酸(11-nor-Δ-THC-COOH)范围内呈线性。15 ng/mL对照品15次重复进样的批内精密度以及161组7、15和60 ng/mL对照品的批间精密度均可接受(变异系数<5.5%)。FGC-MS方法被证明对鉴定11-nor-Δ9-THC-COOH具有特异性,43种测试物质均未干扰11-nor-Δ9-THC-COOH的鉴定和定量。使用两种方法检测的两个标本集的数据一致性良好(R2>0.993)。与传统的气相色谱-质谱联用方法相比,FGC-MS方法可将总检测时间缩短约40%,且数据质量无下降。

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