Liquid-Liquid Extraction Solvent Selection for Comparing Illegal Drugs in Whole Blood and Dried Blood Spot with LC-MS/MS.

IF 2.3 3区医学 Q3 CHEMISTRY, ANALYTICAL

Journal of analytical toxicology Pub Date : 2024-10-05 DOI:10.1093/jat/bkae081

Melike Aydoğdu, Hasan Ertaş, Fatma Nil Ertaş, Serap Annette Akgür

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引用次数: 0

Abstract

Aim: This study focused on the simultaneous detection of amphetamine, 3,4-methyl enedioxy methamphetamine, morphine, benzoylecgonine, and 11-nor-9-carboxy- tetrahydrocannabinol (Δ9-THC-COOH) in whole blood and DBS. It is aimed to select a solvent mixture for liquid-liquid extraction (LLE) technique employing LC-MS/MS. The obtained DBS results were compared with the whole blood samples results.

Methods: A simple, rapid, and reliable LC-MS/MS method was developed and validated for all analytes in whole blood and DBS. LC was performed on a Hypersil Gold C18 column an initial step with a gradient of 0.01 % formic acid, 5 mM ammonium format buffer in water, and acetonitrile at 0.3 ml/min with 7.5-min runtime.

Results: A methanol:acetonitrile (40:60 v/v) mixture was selected for both matrices. LOQ values were 10-25 ng/mL; linear ranges were LOQ-500 ng/ml for all analytes; correlation coefficients were greater than 0.99, and all calibrator concentrations were within 20%. Analytical recovery in blood and DBS ranged from 84.9-113.2% of the expected concentration for both intra and-inter day. Analytes were stable for 1, 10, and 30 days after three freeze/thaw cycles. It was determined that the variances of the results obtained with the two matrices in the comparison study were equal for each analyte, and the results were highly correlated (r=0.9625).

Conclusion: A sensitive, accurate, and reliable chromatographic method was developed to determine amphetamine, MDMA, morphine, benzoylecgonine, and cannabis, by performing the same preliminary steps with whole blood and dried blood spots. It was observed that the results obtained in these two matrices were compatible and interchangeable when statistically compared.

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用 LC-MS/MS 比较全血和干血样中非法药物的液液萃取溶剂选择。

目的：本研究的重点是同时检测全血和 DBS 中的苯丙胺、3,4-甲基烯二氧基甲基苯丙胺、吗啡、苯甲酰可待因和 11-去甲-9-羧基四氢大麻酚（Δ9-THC-COOH）。其目的是为采用 LC-MS/MS 的液液萃取（LLE）技术选择一种混合溶剂。将获得的 DBS 结果与全血样本结果进行比较：方法：针对全血和 DBS 中的所有分析物，开发并验证了一种简单、快速、可靠的 LC-MS/MS 方法。LC 在 Hypersil Gold C18 色谱柱上进行，初始梯度为 0.01 % 甲酸、5 mM 水铵格式缓冲液和乙腈，流速为 0.3 ml/min，运行时间为 7.5 分钟：两种基质均选用甲醇：乙腈（40:60 v/v）混合物。LOQ值为10-25纳克/毫升；所有分析物的线性范围为LOQ-500纳克/毫升；相关系数大于0.99，所有校准物浓度均在20%以内。血液和 DBS 中的分析回收率为日内和日间预期浓度的 84.9%-113.2%。经过三次冻融循环后，分析物在 1 天、10 天和 30 天内都很稳定。在对比研究中，使用两种基质得到的每种分析物的结果方差相等，结果高度相关（r=0.9625）：通过对全血和干血斑进行相同的初步步骤，开发出了一种灵敏、准确、可靠的色谱法，用于测定苯丙胺、摇头丸、吗啡、苯甲酰可待因和大麻。经统计比较发现，在这两种基质中得到的结果是一致的，可以互换。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Journal of analytical toxicology 医学-毒理学

CiteScore

5.10

自引率

20.00%

发文量

审稿时长

6-12 weeks

期刊介绍： The Journal of Analytical Toxicology (JAT) is an international toxicology journal devoted to the timely dissemination of scientific communications concerning potentially toxic substances and drug identification, isolation, and quantitation. Since its inception in 1977, the Journal of Analytical Toxicology has striven to present state-of-the-art techniques used in toxicology labs. The peer-review process provided by the distinguished members of the Editorial Advisory Board ensures the high-quality and integrity of articles published in the Journal of Analytical Toxicology. Timely presentation of the latest toxicology developments is ensured through Technical Notes, Case Reports, and Letters to the Editor.