摘要
建立了一种固相萃取/高效液相色谱-串联质谱(SPE/HPLC-MS/MS)同时检测水体中24种农药的分析方法。样品用乙腈提取后,经固相萃取小柱富集净化。以乙腈-0.1%(体积分数)甲酸水溶液为流动相梯度洗脱,在电喷雾离子源正离子模式下(ESI+)采用多反应监测(MRM)模式检测。结果显示,24种农药在1~200μg/L范围内具有良好的线性关系,相关系数(r2)均不小于0.998,水样中3个添加水平(5、20、100μg/L)下的回收率为65.9%~127.8%,相对标准偏差(RSD)为0.7%~14.2%;方法检出限为0.05~0.71 ng/L。采用该方法对大连地区10个河流入海口及2个水库的水样进行了检测,12个站位的样品中共检出10种农药,质量浓度为0.2~558.3 ng/L。结果表明,所建立的SPE/HPLC-MS/MS方法高效、灵敏、可靠,可用于实际水体中多种农药的同时检测。
A method of solid-phase extraction（SPE） and high performance liquid chromatography-tandem mass spectrometry（SPE/HPLC-MS/MS） was developed for the simultaneous determination of 24 pesticides in water.The samples were extracted with acetonitrile,then enriched and purified with solid-phase extraction cartridges.Acetonitrile and 0.1%（by volume） formic acid aqueous solution were used as mobile phases.Target pesticides were analyzed by HPLC-MS/MS in positive electrospray ionization（ESI＋） under multiple reaction monitoring（MRM） mode.Results showed that 24 pesticides were separated in 25 min with excellent linear relationships（r2≥0.998）.The recoveries at spiked levels of 5,20,100 μg/L in water samples ranged from 65.9%-127.8% with relative standard deviations（RSDs） of 0.7%-14.2%.The limits of detection were in the range of 0.05-0.71 ng/L.This method was applied in the detection of the water samples from 10 estuaries and 2 reservoirs in Dalian,and 10 pesticides were detected in the concentration range of 0.2-558.3 ng/L.The proposed SPE/HPLC-MS/MS method is efficient and sensitive,and is suitable for the determination of various pesticides in actual water samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第12期1487-1493,共7页
Journal of Instrumental Analysis
基金
中央高校基本科研业务费(DUT15LAB04)
关键词
固相萃取
高效液相色谱-串联质谱
农药
水样检测
solid-phase extraction（SPE）
high performance liquid chromatography -tandem massspectrometry（ HPLC - MS/MS）
pesticides
water detection
