在线固相萃取-超高效液相色谱-串联质谱测定饮用水中2,4-滴和灭草松  

Determination of 2,4-D and bentazone in drinking water by on-line SPE-UPLC-MS/MS

作　　者：郑磊 李宏亮[1] 闵巍 詹铭[1] ZHENG Lei;LI Hong-Liang;MIN Wei;ZHAN Ming(Pudong New District Center for Disease Control and Prevention,Shanghai 200136,China)

机构地区：[1]上海市浦东新区疾病预防控制中心,上海200136

出　　处：《实用预防医学》2022年第3期303-306,共4页Practical Preventive Medicine

基　　金：上海市浦东新区卫生系统公共卫生学科建设资助(PWGw2020-04)。

摘　　要：目的建立在线固相萃取-超高效液相色谱-串联质谱测定饮用水中2,4-滴和灭草松的方法。方法水样加入内标后,经微孔滤膜过滤,按水样:纯水=1∶3比例混匀后直接进样,采用在线固相萃取-超高效液相色谱-串联质谱系统进行富集浓缩并测定。样品利用C;固相萃取柱富集浓缩,利用C;色谱柱分离待测物,采用乙腈-水-甲酸为流动相梯度洗脱,负离子模式下,多反应监测模式检测。结果 2,4-滴在5.00~200 ng/L范围内,灭草松在10.0~400 ng/L范围内均有良好的线性关系,线性相关系数(r)>0.9990。检出限分别为2 ng/L和3 ng/L,加标回收率分别为91.2%~95.4%和96.0%~104%。结论该方法操作简单,灵敏快速、准确可靠,适用于饮用水中2,4-滴和灭草松的痕量分析。Objective To establish a method for the determination of 2,4-D and bentazone in drinking water by on-line solid phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry(on-line SPE-UPLC-MS/MS). Methods After adding the internal standard, the water sample was filtered by millipore filtration. The water sample was to be mixed in the proportion of sample water to pure water being 1:3, and then concentrated and detected by on-line SPE-UPLC-MS/MS. The sample was concentrated by SPE on a C;column, separated on a C;column with acetonitrile-water-formic acid as the mobile phase gradient elution, and detected by multiple reaction monitoring(MRM) acquisition under anion mode. Results The linear relationships of 2,4-D and bentazone were good in the ranges of 5.00-200 ng/L and 10.0-400 ng/L,respectively,with the correlation coefficients of more than 0.9990. The method detection limits were 2 ng/L and 3 ng/L,and the recoveries were 91.2%-95.4% and 96.0%-104%,respectively. Conclusion The method is simple,sensitive,rapid,accurate and reliable;and hence,it is applicable to the trace determination of 2,4-D and bentazone in drinking water.

关 键 词：在线固相萃取-超高效液相色谱-串联质谱 2 4-滴 灭草松 饮用水 

分 类 号：R123.1[医药卫生—环境卫生学]