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采用超声辅助低密度溶剂分散液液微萃取-超高效液相色谱-串联质谱法同时测定九种抗凝血灭鼠剂。

Simultaneous determination of nine anticoagulant rodenticides by ultra-performance liquid chromatography-tandem mass spectrometry with ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction.

机构信息

West China School of Basic Medical Sciences and Forensic Medicine, Sichuan University, Chengdu, Sichuan 610000, China.

Department of Traditional Chinese Medicine, Weinan Central Hospital, Weinan 71400, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 15;1092:453-458. doi: 10.1016/j.jchromb.2018.06.053. Epub 2018 Jun 25.

Abstract

A sensitive determination method is developed for nine anticoagulant rodenticides (ARs) in urine samples by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) pretreatment. The target analytes are brodifacoum, bromadiolone, warfarin, coumachlor, coumatetralyl, difenacoum, pindone, diphacinone and chlorophacinone. The parameters that influence the extraction recovery in the UA-LDS-DLLME were systematically investigated and optimized. With the optimized extraction parameters, recoveries ranging from 64.6%-124.2% were obtained for the target analytes. The linear range for all analytes was 0.1-100 ng/mL with correlation coefficients higher than 0.99. Very low LODs ranging in 0.003-0.03 ng/mL were obtained. LOQs were in the range of 0.01-0.1 ng/mL for the nine target analytes. The accuracy that was expressed as mean relative error was within ±5.8% while the precision expressed as relative standard error was less than 5.9%. The combination of UA-LDS-DLLME with UPLC-MS/MS is a feasible, sensitive and rapid analytical approach for the determination of ARs in urine matrix, which is particularly suitable for clinical and forensic purposes.

摘要

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)联用超声辅助低密度溶剂分散液液微萃取(UA-LDS-DLLME)前处理方法,用于尿液样品中九种抗凝杀鼠剂(ARs)的灵敏测定。目标分析物为溴敌隆、溴鼠灵、华法林、氯鼠酮、杀鼠酮、敌鼠、茚满二酮、双苯杀鼠酮和氯鼠酮。系统研究和优化了影响 UA-LDS-DLLME 萃取回收率的参数。在优化的萃取参数下,目标分析物的回收率在 64.6%-124.2%之间。所有分析物的线性范围均为 0.1-100ng/mL,相关系数均高于 0.99。LOD 值均低至 0.003-0.03ng/mL。9 种目标分析物的 LOQs 范围为 0.01-0.1ng/mL。以平均相对误差表示的准确度在±5.8%以内,以相对标准误差表示的精密度小于 5.9%。UPLC-MS/MS 与 UA-LDS-DLLME 的结合是一种用于尿液基质中 ARs 测定的可行、灵敏、快速的分析方法,特别适用于临床和法医用途。

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