固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物  

Simultaneous Determination of Thirty-five Pesticides and Transformation Products in Surface Water Using Solid Phase Extraction Combined with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孙静[1] 徐雄[1] 李春梅[1] 罗茜[1,2] 王东红[1] 王子健[1] 

机构地区：[1]中国科学院生态环境研究中心环境水质学国家重点实验室,北京100085 [2]中国科学院深圳先进技术研究院,深圳518055

出　　处：《分析化学》2015年第8期1145-1153,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No51290283和No21377002)~~

摘　　要：采用固相萃取（SPE）-超高效液相色谱串联质谱（UPLC-MS/MS）技术,建立了同时测定环境水样中痕量浓度多极性的35种高关注农药及转化产物的方法。优化的前处理方法为：串联HLB和活性炭小柱用于富集水样,10 m L乙腈为HLB柱洗脱溶剂,10 m L 20 mmol/L乙酸铵-甲醇作为活性炭柱的洗脱溶剂,将洗脱溶液混合、浓缩、溶剂转化和定容,定容溶剂为10 mmol/L乙酸铵的乙腈-水的混合溶液（1∶1,V/V）。流动相分别为5 mmol/L甲酸铵-甲酸缓冲溶液（p H 3.5）和乙腈进行UPLC色谱分离,质谱用多反应监测（MRM）模式进行分析测定。实验结果表明,目标物在0.5~200μg/L含量范围内线性良好（R2≥0.9802）,检出限范围为0.01~0.8 ng/L,回收率在60%~120%之间。本研究构建的SPE-UPLC-MS/MS方法灵敏可靠,可用于对地表水中ng/L级极性不同的多种农药及转化产物的测定。A method based on solid phase extraction combined with ultra-performance liquid chromatography- tandem mass spectrometry （SPE-UPLC-MS/MS） was established for the simultaneous determination of thirty-five pesticides and transformation products of high concern with different polarities at trace level in environmental waters. Under optimized conditions, tandem cartridges with Oasis HLB column and activated carbon were used for the enrichment of water samples. HLB column was eluted by 10 mL of acetonitrile, and activated carbon cartridge was eluted by 10 mL of methanol solution containing 20 mmol/L ammonium acetate. The elution solvents were mixed, concentrated and reconstituted. Finally, the elution solvent was reconstituted with a mixed solution of acetonitrile and water （ 1 ： 1, V/V） containing 10 mmol/L ammonium acetate. The targets were separated by gradient elution with 5 mmol/L ammonium formate buffer and acetonitrile as mobile phases, and detected by MS/MS in the multi-reactions monitoring （MRM） mode. Under the experimental conditions, good linearity ranging from 0.5-200 μg/L was made （R2≥0. 9802）, and the limits of detection （LODs） were from 0.01 ng/L to 0.8 ng/L. Recoveries of most targets were 60%-120%. The SPE-UPLC- MS/MS method established here is reliable and can be applied to determine ng/L level of pesticides and transformation products with different polarities in surface water.

关 键 词：农药 转化产物 固相萃取 超高效液相色谱-串联质谱法 地表水 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]