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应用固相萃取-超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)联用技术,建立了水中20种菊酯类农药多残留的分析方法。通过对固相萃取柱、淋洗液、流动相等条件的优化,确定以Oasis HLB为固相萃取柱、正己烷-丙酮(9∶1,V/V)为淋洗液、0.1%乙酸水溶液-乙腈(7∶3,V/V)为流动相做水样预处理。在最优实验条件下,目标物的回收率为73.4%~124.5%,相对标准偏差(RSD)在5.7%9.1%之间,线性范围均在12 000μg/L,各目标物标准品在UPLC-MS/MS系统中有效的线性相关(R2)为0.999以上。该方法具有检测限低、回收率高等优点,经实际样品测试,可适用于水中20种菊酯类农药多残留的同时检测。
Abstract：An analytical method for simultaneous determination of 20 pyrethroid pesticides in water samples was developed by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometer(UPLC-MS/MS).Oasis HLB solid phase extraction column,hexane-acetone(9∶1,V/V)as washing solution,0.1% acetic acid-acetamide(7∶3,V/V)as the mobile phase were selected for sample pretreatment and chromatography separation.Based on the optimized sample pretreatment procedures and separation condition,the target recoveries ranged from 73.4% to 124.5%in water with the relative standard deviations(RSDs)from 5.7% to 9.1%.The linear ranges were from 1to 2 000μg/L with correlation coefficients(R2)not less than 0.999.The method can be applied to simultaneous determination of 20 pyrethriod pesticides in surface water owing to the low detection limit and high recovery.
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基本信息:
DOI：10.13526/j.issn.1006-6144.2017.01.012
中图分类号:TQ450.263;O657.63
引用信息:
[1]吴春英,谷风,白鹭,等.固相萃取-超高效液相色谱-三重四极杆质谱联用同时测定水中菊酯类农药多残留[J].分析科学学报,2017,33(01):57-62.DOI:10.13526/j.issn.1006-6144.2017.01.012.
基金信息:
中国博士后科学基金(No.20080440374)
2017-02-27
2017-02-27
2017-02-27