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同时测定六种新型精神活性物质的超高效液相色谱-质谱联用方法的建立与验证

Development and validation of the UPLC-MS method for simultaneous determination of six new psychoactive substances.

作者信息

Tan Zhouhong, Wen Yunbo, Yang Kai, Zhao Xia, Yang Xiaoli, He Jieli

机构信息

College of Pharmacy, Dali University Dali 671000 Yunnan P. R. China

Yunnan Provincial Key Laboratory of Forensic Science Kunming 650223 Yunnan P. R. China.

出版信息

RSC Adv. 2022 Sep 21;12(41):26704-26711. doi: 10.1039/d2ra04869h. eCollection 2022 Sep 16.

DOI:10.1039/d2ra04869h
PMID:36320845
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9490772/
Abstract

The combined abuse of benzodiazepines and antipsychotics has become a global problem, and to develop a highly sensitive and selective method for monitoring of benzodiazepine hypnotics and antipsychotics is urgently necessary. In this work, we established a rapid method for the simultaneous determination of benzodiazepines (diazepam, alprazolam, triazolam, and estazolam) and antipsychotic drugs (clozapine, and chlorpromazine) based on ultra performance liquid chromatography-mass spectrometry (UPLC-MS). The accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), specificity, matrix effect and carry-over effect were verified in detail. The results of the recovery and repeat experiments proved that the proposed UPLC-MS method possessed very satisfactory accuracy and precision. The LOD and LOQ of the six psychoactive substances were as low as 0.001-0.005 and 0.005-0.01 μg L, respectively. The proposed method was employed to analyze urine samples which were pretreated with a protein precipitation process. The potential influences of precipitants on the analysis results were evaluated statistically, and 0.1% formic acid/acetonitrile/water was selected as the optimum precipitation agent. The detection of the targets was free from matrix and carryover effects.

摘要

苯二氮䓬类药物和抗精神病药物的联合滥用已成为一个全球性问题,因此迫切需要开发一种高灵敏度和高选择性的方法来监测苯二氮䓬类催眠药和抗精神病药物。在本研究中,我们基于超高效液相色谱-质谱联用(UPLC-MS)建立了一种同时测定苯二氮䓬类药物(地西泮、阿普唑仑、三唑仑和艾司唑仑)和抗精神病药物(氯氮平和氯丙嗪)的快速方法。详细验证了该方法的准确性、精密度、检测限(LOD)、定量限(LOQ)、特异性、基质效应和残留效应。回收率和重复性实验结果表明,所建立的UPLC-MS方法具有非常令人满意的准确性和精密度。六种精神活性物质的检测限和定量限分别低至0.001 - 0.005和0.005 - 0.01 μg/L。该方法用于分析经蛋白沉淀法预处理的尿液样本。对沉淀剂对分析结果的潜在影响进行了统计学评估,选择0.1%甲酸/乙腈/水作为最佳沉淀剂。目标物的检测不受基质和残留效应的影响。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/2f62b6d37952/d2ra04869h-f3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/0173d17f0ef2/d2ra04869h-f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/bbaa83ee3822/d2ra04869h-f2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/2f62b6d37952/d2ra04869h-f3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/0173d17f0ef2/d2ra04869h-f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/bbaa83ee3822/d2ra04869h-f2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7f09/9490772/2f62b6d37952/d2ra04869h-f3.jpg

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