色谱Issue(7)：691-698,8.DOI:10.3724/SP.J.1123.2015.03010
在线固相萃取／液相色谱-线性离子阱质谱法同时定性定量检测全血和尿液中7种抗凝血杀鼠药
Simultaneous qualitative and quantitative determination of seven anticoagulant rodenticides in whole blood and urine samples using on-line solid phase extraction with liquid chromatography-linear ion trap mass spectrometry
黄克建 1李宏森 1李璐 1黄晓青 1卢敏萍 2周哲 3林翠梧 2杨宁 1刘晓锋 1朱定姬 4梁平 1乔文涛1
作者信息
- 1. 广西壮族自治区公安厅物证鉴定中心，广西 南宁 530012
- 2. 广西大学化学化工学院，广西 南宁 530004
- 3. 赛默飞世尔科技 中国 有限公司，上海 201206
- 4. 广西壮族自治区职业病防治研究院，广西 南宁 530021
- 折叠
摘要
Abstract
A new and sensitive analytical method has been developed for the simultaneous determination of seven anticoagulant rodenticides in whole blood and urine samples by liquid chromatography-linear ion trap mass spectrometry ( LC-LIT/MS ) with on-line solid phase extraction( on-line SPE). The samples were treated with acetonitrile,followed by dilution, centrifugation,and filtration. The resulting solution was injected into the LC system directly and processed by on-line SPE column for enrichment and purification. Separation was performed on a C18 column with mixed mobile phases of methanol and 0. 02 mol/L ammonium acetate aque-ous solution for gradient elution. The analytes were detected by the mass spectrometer with electrospray ionization(ESI)in negative mode. MS2 full scan signals of the target parent ions within the locked retention time window were recorded. Self-built database searching was performed for qualitative confirmation,and MS2 fragment ions with high sensitivity and specific-ity were selected for quantification. Simultaneous qualitative and quantitative analyses of the seven rodenticides were achieved in this way. Good linearities were obtained within the investi-gated mass concentration ranges of the seven rodenticides,with r2≥0. 995 8 in blood and r2≥0. 994 6 in urine. The LODs varied from 0. 02 ng/mL to 1. 00 ng/mL,and the LOQs varied from 0. 10 ng/mL to 4. 00 ng/mL. The recoveries at three spiked levels in blood and urine samples ranged from 81. 0% to 113. 9%,with RSDs of 0. 1%-6. 2%( n=6 ). The developed method is simple,sensitive,and can be used for the rapid detection and accurate quantification of the seven anticoagulant rodenticides in whole blood and urine samples.关键词
在线固相萃取/液相色谱-线性离子阱质谱法/抗凝血杀鼠药/全血/尿液Key words
on-line solid phase extraction( on-line SPE )/liquid chromatography-linear ion trap mass spectrometry( LC-LIT/MS)/anticoagulant rodenticides/whole blood/urine分类
化学化工引用本文复制引用
黄克建,李宏森,李璐,黄晓青,卢敏萍,周哲,林翠梧,杨宁,刘晓锋,朱定姬,梁平,乔文涛..在线固相萃取／液相色谱-线性离子阱质谱法同时定性定量检测全血和尿液中7种抗凝血杀鼠药[J].色谱,2015,(7):691-698,8.
