摘要
为了更准确的检测氨基甲酸酯类农药在地表水中的残留水平,建立了无需前处理,直接进样快速测定氨基甲酸酯类农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经0.2μm针式滤头过滤除去颗粒性杂质后,UPLC-MS/MS进样分析,采用Waters Acquity Uplctm BEH C18色谱柱,甲醇和5mM乙酸铵水溶液作为流动相进行梯度洗脱,电喷雾离子源电离,正离子多反应监测模式进行定性和定量分析。20种氨基甲酸酯类农药在0.10～100μg/L浓度范围内线性关系良好,相关系数r在0.995 6～0.999 7之间,方法的检出限为0.01～0.05μg/L;高、中、低3个添加水平的回收率为72.2%～117%,相对标准偏差在1.82%～14.2%之间。结果表明,该方法灵敏、准确且检测范围广、分析速度快。
A method without any pre-treatment steps using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry （UPLC-MS/MS） was developed and applied for the rapid determination of carbamate residues in surface water. Water sample was filtered with 0.2μm syringe filter for particle removal and injected directly into UPLC, and separation was performed on an Aequity Uplctm BEH C18 column utilizing a gradient elution program of methnol and water （containing 5 mM ammonium acetate） as the mobile phase. Identification and quantification were achieved by UPLC-ESI-MS/MS in positive mode and multiple reactions monitoring （MRM）. Good linearity was observed in the range of 0.10-100 μg/L with correlation coefficients from 0. 995 6 to 0. 999 7,limit of detection （LOD） for the 20 carbamates was in the ranges of 0. 01-0. 05 μg/L. The recoveries ranged from 72.2% to 117% with the relative standard deviations were between 1. 82% and 14.2%. The method is characterized by high sensation and precision, extensive analytical range and quick analytical rate.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2012年第3期175-180,共6页
Journal of Chinese Mass Spectrometry Society
基金
杭州市环境保护科技项目(2011003)
杭州市科技发展计划项目(20100933B37)资助
作者简介
张明（1981～），男（汉），浙江三门人，硕士，从事环境监测方法研究。E—mail：zjuzhang@gmail．com
