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超高效液相色谱-串联质谱法检测干血斑中的合成卡西酮及其代谢物。

Screening of Synthetic Cathinones and Metabolites in Dried Blood Spots by UPLC-MS-MS.

机构信息

School of Pharmacy, Fudan University, Shanghai 200032, China.

Department of Forensic Toxicology, Academy of Forensic Science, Shanghai Key Laboratory of Forensic Medicine, Guangfu Xi Road 1347, Shanghai 200063, China.

出版信息

J Anal Toxicol. 2021 Aug 14;45(7):633-643. doi: 10.1093/jat/bkaa106.

Abstract

After its use for decades in clinical screening, dried blood spots (DBS) have recently received considerable attention for their application in various novel psychoactive substances. The goal of this study was to develop and apply a DBS-based assay for 37 synthetic cathinones and their metabolites. Thirty microliters of whole blood sample after administration was spotted onto Whatman FTA classical cards, dried and extracted, and then analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). The samples were chromatographed on a Waters Acquity UPLC®HSS T3 column (1.8 μm, 2.1 × 100 mm) and then identically packed defender guard cartridges of a Waters Acquity UPLC®HSS T3 column (1.8 μm, 2.1 × 5 mm, 3/pk). The separation was achieved via solvents of 20 mM ammonium acetate/formic acid 0.1% (A) and acetonitrile (B) at a flow rate of 0.25 mL/min. A tandem MS equipped with positive electrospray ionization mode source was used as the detector. Multiple reaction monitoring with the precursor/product ion combinations was used to quantify each analyte. The linear range of synthetic cathinones in the DBS was 2.0-200 ng/mL, and the lowest limit of quantification was 2.0 ng/mL for some synthetic cathinones and 10 ng/mL for others. The precision and accuracy of the results for the validation samples of the synthetic cathinones were within acceptable criteria. DBS sampling offers the advantages of reduced sample volume and convenient sample storage and shipment. This method can be successfully applied to the quantification of synthetic cathinones.

摘要

经过数十年的临床筛查应用,干血斑(DBS)最近因其在各种新型精神活性物质中的应用而受到广泛关注。本研究旨在开发和应用一种基于 DBS 的方法来检测 37 种合成苯丙胺类兴奋剂及其代谢物。给药后采集 30 μL 全血样本,点样于 Whatman FTA 经典卡上,干燥后提取,然后用超高效液相色谱-串联质谱法(UPLC-MS-MS)分析。样品在 Waters Acquity UPLC®HSS T3 柱(1.8 μm,2.1 × 100 mm)上进行色谱分离,然后使用 Waters Acquity UPLC®HSS T3 柱(1.8 μm,2.1 × 5 mm,3 个/包)的相同保护柱进行分离。通过 20 mM 乙酸铵/甲酸 0.1%(A)和乙腈(B)作为溶剂以 0.25 mL/min 的流速实现分离。串联质谱采用正电喷雾电离源作为检测器。采用母离子/子离子组合的多反应监测模式进行定量分析。DBS 中合成苯丙胺类兴奋剂的线性范围为 2.0-200 ng/mL,部分合成苯丙胺类兴奋剂的定量下限为 2.0 ng/mL,其他合成苯丙胺类兴奋剂的定量下限为 10 ng/mL。合成苯丙胺类兴奋剂验证样本的精密度和准确度均符合可接受标准。DBS 采样具有减少样本量、方便样本储存和运输的优点。该方法可成功应用于合成苯丙胺类兴奋剂的定量检测。

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