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GC-MS analysis of underivatised new psychoactive substances in whole blood and urine
Journal of Chromatography B ( IF 3 ) Pub Date : 2020-08-11 , DOI: 10.1016/j.jchromb.2020.122308
Anastasia Alexandridou , Thomai Mouskeftara , Nikolaos Raikos , Helen G. Gika

Herein a method was develop and validated for the detection and quantification of five new psychoactive substances (NPS) belonging to three categories: synthetic cathinones (mephedrone, 3,4-MDPV), opioids (AH-7921) and cannabinoids (JWH-018, AM-2201) by EI GC-MS. Target analytes were quantified in whole blood; in urine the same compounds plus methylone were detected. Liquid-liquid extraction by MTBE - butyl acetate (1:1, v/v) in blood and butyl acetate in urine was applied for the recovery of analytes, while no derivatization was necessary for their sensitive detection and quantification. The method showed good linearity for all analytes within a concentration range from 0.25 to 2 μg/mL for mephedrone, from 0.02 to 0.16 μg/mL for 3,4-MDPV and AH-7921 and from 0.005 to 0.04 μg/mL for JWH-018 and AM-2201. LOD ranged from 0.002 μg/mL (JWH-018 and AM-2201 in blood and urine), to 0.08 μg/mL (mephedrone in urine). LOQ in blood ranged from 0.005 μg/mL for JWH-018 and AM-2201 to 0.25 μg/mL for mephedrone. Accuracy was within acceptable limits with % bias ranging from +20% to -17.98% for intra-assay study and from +18.87% to -11.16% for inter-assay study. Precision was found to be between 2.60% and 17.17% (CV%) for intra-assay study and from 6.03% to 13.72% (CV%) for inter-assay study. An intra laboratory comparison provided proof of the method robustness. The developed method can be used for the reliable and fast quantification of five NPS in blood and the detection of six NPS in urine within the practice of a clinical or forensic toxicology laboratory.



中文翻译:

GC-MS分析全血和尿液中已消失的新型精神活性物质

本文开发并验证了一种方法,用于检测和定量五种新的精神活性物质(NPS),这些物质属于三类:合成的卡西酮(甲基吗啡酮,3,4-MDPV),阿片类药物(AH-7921)和大麻素(JWH-018, EI GC-MS)。在全血中对目标分析物进行定量;尿液中检测到相同的化合物和甲酮。通过MTBE液-液萃取-血液中的乙酸丁酯(1:1,v / v)和尿液中的乙酸丁酯用于回收分析物,而无需衍生化即可灵敏地检测和定量分析物。该方法对所有分析物均表现出良好的线性,对甲氧麻黄酮的浓度范围为0.25至2μg/ mL,对3,4-MDPV和AH-7921为0.02至0.16μg/ mL,对JWH-为0.005至0.04μg/ mL 018和AM-2201。LOD范围为0。002μg/ mL(血液和尿液中的JWH-018和AM-2201)至0.08μg/ mL(尿液中的甲吗啡酮)。血液中的LOQ范围从JWH-018和AM-2201的0.005μg/ mL到甲氧麻黄酮的0.25μg/ mL。批内分析的准确性在可接受的范围内,偏差百分比范围为+ 20%至-17.98%,而批间分析的准确性偏差为+ 18.87%至-11.16%。批内研究的精密度在2.60%和17.17%(CV%)之间,批间研究的精密度在6.03%至13.72%(CV%)之间。实验室内部的比较提供了方法稳健性的证明。在临床或法医毒理学实验室的实践中,开发的方法可用于可靠,快速地定量血液中的五种NPS,并检测尿液中的六种NPS。对于JWH-018和AM-2201,为005μg/ mL,对于甲氧麻黄酮为0.25μg/ mL 批内分析的准确性在可接受的范围内,偏差百分比范围为+ 20%至-17.98%,而批间分析的准确性偏差为+ 18.87%至-11.16%。批内研究的精密度在2.60%和17.17%(CV%)之间,批间研究的精密度在6.03%至13.72%(CV%)之间。实验室内部的比较提供了方法稳健性的证明。所开发的方法可用于在临床或法医毒理学实验室的实践中对血液中5种NPS进行可靠,快速的定量,并在尿液中检测6种NPS。对于JWH-018和AM-2201,为005μg/ mL,对于甲氧麻黄酮为0.25μg/ mL。批内分析的准确性在可接受的范围内,偏差百分比范围为+ 20%至-17.98%,而批间分析的偏差百分比为+ 18.87%至-11.16%。批内研究的精密度在2.60%和17.17%(CV%)之间,批间研究的精密度在6.03%至13.72%(CV%)之间。实验室内部的比较提供了方法稳健性的证明。所开发的方法可用于在临床或法医毒理学实验室的实践中对血液中5种NPS进行可靠,快速的定量,并在尿液中检测6种NPS。批内研究的结果为17%(CV%),批间研究的数据为6.03%至13.72%(CV%)。实验室内部的比较提供了方法稳健性的证明。所开发的方法可用于在临床或法医毒理学实验室的实践中对血液中5种NPS进行可靠,快速的定量,并在尿液中检测6种NPS。批内研究的结果为17%(CV%),批间研究的数据为6.03%至13.72%(CV%)。实验室内部的比较提供了方法稳健性的证明。所开发的方法可用于在临床或法医毒理学实验室的实践中对血液中5种NPS进行可靠,快速的定量,并在尿液中检测6种NPS。

更新日期:2020-08-11
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