溶剂诱导萃取/UPLC-MS/MS法高通量检测环境水体中12种除草剂

High Throughput Detection of 12 Herbicides in Environmental Water by UPLC-MS/MS Method with Solvent Induced Extraction

以二氯甲烷为萃取剂,建立了测定环境水样中12种除草剂的溶剂诱导萃取/超高效液相色谱-串联质谱(UPLC-MS/MS)法。通过单因素实验确定提取剂乙腈的体积、萃取剂的种类和体积、离心时间,并结合响应面分析,得到最优的前处理方法;在仪器方法建立过程中对质谱参数、色谱柱、流动相进行了优化。在最优条件下,12种除草剂的线性关系良好,相关系数(r)均大于0.999 5,方法检出限为0.05~0.5μg/L,定量下限为0.2~5.0μg/L,平均回收率为83.0%~110%,相对标准偏差为0.30%~5.0%。该方法简便快捷、灵敏度高、有机溶剂用量少,适用于环境水体中除草剂的高通量检验。

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with dichloromethane solvent induced extraction was established for the determination of 12 herbicides in environmental water.The volume of extractant acetonitrile,the type and dosage of extractant,and the centrifugation time were determined by single factor test.Combined with response surface analysis,an optimal pretreatment method was obtained.Meanwhile,mass spectrum parameters,chromatographic column and different mobile phases were also optimized during the establishment of the instrument method.Under the optimal conditions,the calibration curves for 12 herbicides were in good linear relationships,with their correlation coefficients(r) greater than 0. 999 5.The limits of detection and the limits of quantitation were in the ranges of 0. 05-0. 5 μg/L and 0. 2-5. 0 μg/L,respectively.Average recoveries ranged from 83. 0% to 110%,with relative standard deviations of 0. 30%-5. 0%.The method is simple,sensitive and low organic solvent consumption,and it is suitable for the high throughput inspection of actual samples.