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.
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.
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.
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。