分析测试学报2018，Vol.37Issue(1)：1-9,9.DOI:10.3969/j.issn.1004-4957.2017.01.001
在线固相萃取/液相色谱-串联质谱法快速检测全血及尿液中15种杀鼠药
Analysis of Fifteen Rodenticides in Whole Blood and Urine Samples by Liquid Chromatography-Tandem Mass Spectrometry with On-line Solid Phase Extraction
摘要
Abstract
A analytical method was developed for the simultaneous determination of fifteen rodenticides in whole blood and urine samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with on-line solid phase extraction (on-line SPE).The samples were treated with acetonitrile,followed by dilution,centrifugation and filtration.The solution obtained was purified with a polymer column for hydrophilic-lipophilic balance (HLB),then eluted on a ZORBAX Eclipse Plus C18 column with acetonitrile and 0.01 mol/L ammonium acetate aqueous solution as mobile phase.The analytes were detected in dynamic multiple reaction monitoring (DMRM) mode under alternate positive/negative electrospray ionization (ESI+/ESI-) mode,and quantified by external standard method.The results showed that there existed good linear relationships by quadratic equation fitting for the fifteen rodenticides in whole blood and urine in the investigated mass concentration ranges with the correlation coefficients not less than 0.997 8 for whole blood and not less than 0.996 5 for urine,respectively.The LODs and the LOQs varied from 0.10 μg/L to 5.00 μg/L and 0.50 μg/L to 10.0 μg/L,respectively.The recoveries at three spiked levels in whole blood and urine ranged from 81.8％ to 109.6％ with their RSDs of 0.3％-3.8％ (n =6).The developed method is simple and reliable,and is sensitive for the rapid detection and accurate quantification of fifteen rodenticides in whole blood and urine samples.关键词
在线固相萃取/液相色谱-串联质谱/杀鼠药/血液/尿液/二次方程Key words
on-line solid phase extraction (on-line SPE)/liquid chromatography-tandem mass spectrometry (LC-MS/MS)/rodenticides/whole blood/urine/quadratic equation分类
化学化工引用本文复制引用
黄克建,梁平,易叶平,刘慧,侯笑然,莫静,刘晓锋,杨宁,罗轩,朱定姬,李璐,乔文涛,黄晓青..在线固相萃取/液相色谱-串联质谱法快速检测全血及尿液中15种杀鼠药[J].分析测试学报,2018,37(1):1-9,9.基金项目
广西公安科学研究与技术开发计划立项项目(GAT2016-14) （GAT2016-14）
