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Simultaneous Determination of Eighteen Carbamate Pesticides in Biological Samples by On-line Solid Phase Extraction Coupled with Liquid Chromatography-Linear Ion Trap Mass Spectrometry |
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DOI: |
KeyWord:on-line solid phase extraction(on-line SPE) liquid chromatography-linear ion trap mass spectrometry(LC-LIT/MS) consecutive reaction monitoring(CRM) carbamate pesticides biological samples |
Author | Institution |
LU Min-ping,HUANG Ke-jian,ZHOU Zhe,LIN Cui-wu*,YANG Ning,LIU Xiao-feng,GAO Fan-qin |
1.广西大学化学化工学院;2.广西壮族自治区公安厅物证鉴定中心;3.赛默飞世尔科技中国有限公司;4.广西高校应用化学技术与资源开发重点实验室;5.西安力邦医药科技有限责任公司 |
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Abstract: |
A new and sensitive analytical method was developed for the simultaneous determination of eighteen carbamate pesticides in biological samples by on-line solid phase extraction(on-line SPE) coupled with liquid chromatography-linear ion trap mass spectrometry(LC-LIT/MS).The samples were treated with acetonitrile,followed by dilution and centrifugation.The resulting solution was injected into LC system directly and processed with an Waters Oasis? HLB On-line SPE column for enrichment and purification.Separation was performed on a BETASIL C18 column with mixed mobile phases of methanol and water(both containing 0.1% formic acid) by gradient elution.The analytes were detected in selected reaction monitoring(SRM) or consecutive reaction monitoring(CRM) mode through positive electrospray ionization(ESI+).The calibration curves were linear within the investigated mass concentration ranges of the analytes(weighted 1/X),with correlation coefficients(r2) of 0.9943-0.9994.The LODs were in the ranges of 0.1-5ng/mL for whole blood and urine,and 0.1-5ng/g for liver tissue.The recoveries at three spiked levels ranged from 90.2% to 114.5%,with RSDs(n=4) of 0.5%-7.5%.The developed method is simple and accurate,and is sensitive for the rapid determination of eighteen carbamate pesticides in biological samples. |
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