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分析化学  2015 

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

DOI: 10.11895/j.issn.0253-3820.150208, PP. 1145-1153

Keywords: 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

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Abstract:

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,10mL乙腈为HLB柱洗脱溶剂,10mL20mmol/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10mmol/L乙酸铵的乙腈-水的混合溶液(1:1,V/V)。流动相分别为5mmol/L甲酸铵-甲酸缓冲溶液(pH3.5)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0.01~0.8ng/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。

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