| 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 |
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| 作者 | 单位 | | 黄克建，莫静,刘晓锋,杨宁,罗轩,朱定姬,李璐,乔文涛,黄晓青,梁平,易叶平,刘慧,侯笑然 | 1.广西壮族自治区公安厅物证鉴定中心；2.广西大学化学化工学院；3.广西壮族自治区职业病防治研究院 |
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| 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) |
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| 中文摘要:建立了同时测定血液和尿液样品中15种杀鼠药的在线固相萃取/液相色谱-三重四极杆串联质谱(On-line SPE/LC-MS/MS)分析方法。用乙腈沉淀样品中的蛋白质，经稀释、离心、过滤后直接进样。通过在线固相萃取柱HLB富集纯化，以ZORBAX Eclipse Plus C18柱为分析柱，乙腈-0.01 mol/L乙酸铵水溶液为流动相进行梯度洗脱。采用电喷雾电离(ESI+/ESI-)快速正负切换模式，动态多反应监测模式(DMRM)扫描，外标法定量。结果表明，15种杀鼠药采用二次方程拟合时线性关系良好，血液中r2≥0.997 8，尿液r2≥0.996 5，方法的检出限和定量下限分别为0.10~5.00 μg/L和0.50~10.0 μg/L，3个添加水平下的回收率为81.8%~109.6%，日内相对标准偏差(RSD)为0.3%~3.6%，日间RSD为0.3%~3.8% (n =6)。该方法简单方便，灵敏度高，能够用以血液和尿液样品中15种杀鼠药的快速筛查和准确定量。 |
| 中文关键词: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 |
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| Analysis of Fifteen Rodenticides in Whole Blood and Urine Samples by Liquid Chromatography-Tandem Mass Spectrometry with On-line Solid Phase Extraction |
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| 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. |
| Key Words:on-line solid phase extraction(on-line SPE) liquid chromatography-tandem mass spectrometry(LC-MS/MS) rodenticides whole blood urine quadratic equation |
| 引用本文：黄克建，莫静,刘晓锋,杨宁,罗轩,朱定姬,李璐,乔文涛,黄晓青,梁平,易叶平,刘慧,侯笑然.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. |
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