高通量液相色谱-真空微分迁移谱-质谱法分析人体尿液中的异构体滥用药物。

IF 2.6 3区 医学 Q2 BIOCHEMICAL RESEARCH METHODS Drug Testing and Analysis Pub Date : 2024-07-31 DOI:10.1002/dta.3778
Maria Fernanda Cifuentes Girard, Patrick Knight, Gérard Hopfgartner
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引用次数: 0

摘要

研究了低压差示迁移率光谱法与液相色谱-质谱联用技术(LC-vDMS-MS)在 13 种滥用药物(DoA)分析中的应用,包括以下药物:可卡因、埃可宁甲酯、古柯碱、苯甲酰埃可宁、诺可卡因、曲马多、代谢物异构体对;O-去甲基-顺式曲马多和 N-去甲基-顺式曲马多以及大麻素:Δ9-四氢大麻酚、Δ9-四氢大麻酚、11-羟基-Δ9-四氢大麻酚、11-去甲-9-羧基-Δ9-四氢大麻酚和 11-去甲-9-羧基-Δ9-四氢大麻酚葡萄糖醛酸内酯。对异构体分离的不同参数进行了优化,如 LC 流动相组成(20%-100% 甲醇乙腈和异丙醇,流速:8-100 μL/min )和 DMS 分离电压。甲醇和乙腈会明显影响分析物的补偿电压,并改善 DMS 分离效果。除了用 4 分钟的 LC-vDMS-SIM/MS 方法鉴定和定量五种大麻素(包括异构体 THC/CBD 和三种 THC 代谢物)之外,还开发了一种 1 分钟的短捕集/静置 LC-vDMS-SIM/MS 筛选方法,用于定量 11 种滥用药物(THC/CBD 除外)。四氢大麻酚是大麻的主要精神活性成分,与其同分异构体 CBD 相比,四氢大麻酚是一种受管制物质;这凸显了通过分析技术解决这些异构体对的重要性和挑战性。在 0.005-10 μg/mL 的浓度范围内,DoA 的信号响应呈线性;在 1-1000 ng/mL 的浓度范围内,大麻素的信号响应呈线性。日内和日间精确度优于 12.2%,准确度优于 115%。对路边药物检测中四氢大麻酚和/或可卡因检测呈阳性的受试者的尿样进行了评估,以评估 LC-vDMS-SIM/MS 和 LC-MRM/MS 方法的性能。结果表明,所开发的 LC-vDMS-SIM/MS 方法与 LC-MRM/MS 性能相似,但样品处理量有所提高。
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High-throughput liquid chromatography-vacuum differential mobility spectrometry-mass spectrometry for the analysis of isomeric drugs of abuse in human urine.

The use of differential mobility spectrometry at low pressure coupled to liquid chromatography-mass spectrometry (LC-vDMS-MS) was investigated for the analysis of 13 drugs of abuse (DoA) including the following: cocaine, ecgonine methyl ester, cocaethylene, benzoylecgonine, norcocaine, tramadol, isomeric pairs of metabolites; O-desmethyl-cis-tramadol and N-desmethyl-cis-tramadol, and cannabinoids: Δ9-tetrahydrocannabinol, Δ9-tetrahydrocannabidiol, 11-hydroxy-Δ9-tetrahydrocannabinol, 11-nor-9carboxy-Δ9-tetrahydrocannabinol, and 11-nor-9carboxy-Δ9-tetrahydrocannabinol glucuronide. Different parameters were optimized for isomeric separation, such as LC mobile phase composition (20%-100% methanol acetonitrile and isopropanol, flow rate: 8-100 μL/min) and DMS separation voltage. Methanol and acetonitrile significantly affected the compensation voltage of the analytes and improved DMS separation. A short trap/elute LC-vDMS-SIM/MS screening method of 1 min was developed to quantify 11 drugs of abuse (except THC/CBD), in addition to a 4-min LC-vDMS-SIM/MS method to identify and quantify five cannabinoids including the isomers THC/CBD and three THC metabolites. THC is the principal psychoactive constituent of cannabis and is a controlled substance in comparison to its isomeric counterpart CBD; this highlights the importance and challenges to resolve these isomeric pairs by analytical techniques. The signal responses were linear over a concentration range of 0.005-10 μg/mL for the DoA and 1-1000 ng/mL for cannabinoids. The intraday and interday precision were better than 12.2% and accuracy better than 115%. Urine samples from subjects who tested positive for THC and/or cocaine during roadside drug testing were evaluated to assess the performance of the methods LC-vDMS-SIM/MS and LC-MRM/MS. Results show that the developed LC-vDMS-SIM/MS method presents similar performance to LC-MRM/MS with improved sample throughput.

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来源期刊
Drug Testing and Analysis
Drug Testing and Analysis BIOCHEMICAL RESEARCH METHODS-CHEMISTRY, ANALYTICAL
CiteScore
5.90
自引率
24.10%
发文量
191
审稿时长
2.3 months
期刊介绍: As the incidence of drugs escalates in 21st century living, their detection and analysis have become increasingly important. Sport, the workplace, crime investigation, homeland security, the pharmaceutical industry and the environment are just some of the high profile arenas in which analytical testing has provided an important investigative tool for uncovering the presence of extraneous substances. In addition to the usual publishing fare of primary research articles, case reports and letters, Drug Testing and Analysis offers a unique combination of; ‘How to’ material such as ‘Tutorials’ and ‘Reviews’, Speculative pieces (‘Commentaries’ and ‘Perspectives'', providing a broader scientific and social context to the aspects of analytical testing), ‘Annual banned substance reviews’ (delivering a critical evaluation of the methods used in the characterization of established and newly outlawed compounds). Rather than focus on the application of a single technique, Drug Testing and Analysis employs a unique multidisciplinary approach to the field of controversial compound determination. Papers discussing chromatography, mass spectrometry, immunological approaches, 1D/2D gel electrophoresis, to name just a few select methods, are welcomed where their application is related to any of the six key topics listed below.
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