QuEChERS-超高效液相色谱-串联质谱法测定不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂

Simultaneous determination of 11 strobilurin fungicides in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

建立了同时检测6种不同植被类型土壤中11种甲氧基丙烯酸酯类杀菌剂(丁香菌酯、氯啶菌酯、啶氧菌酯、氟嘧菌酯、肟菌酯、E-苯氧菌胺、醚菌酯、醚菌胺、肟醚菌胺、唑菌酯和烯肟菌胺)的Qu ECh ERS-超高效液相色谱-串联质谱分析方法。土壤样品经0.1%(体积分数)醋酸乙腈提取,用100 mg N-丙基乙二胺(PSA)和100 mg C18净化。采用C18色谱柱进行色谱分离和分析,以甲醇和水为流动相进行梯度洗脱,以电喷雾正离子、多反应监测模式进行定性分析,采用基质标准曲线外标法进行定量分析。结果表明:11种甲氧基丙烯酸酯杀菌剂在0.1~100μg/kg范围内线性关系良好,相关系数为0.980 5~0.999 9。空白样品在5、10和50μg/kg添加水平下的平均回收率为65.1%~103.9%,相对标准偏差为0.082%~14%(n=3),定量限为0.005~2.0μg/kg。该方法能够满足不同植被类型土壤(黑土、红壤土、砂土、潮土、灰漠土、高山土)中11种甲氧基丙烯酸酯类杀菌剂痕量检测的要求。

A method for the simultaneous determination of the 11 strobilurin fungicides(coumoxystrobin,tricyclopyricarb,picoxystrobin,fluoxastrobin,trifloxystrobin,E-metominostrobin,kresoxim-methyl,dimoxystrobin,orysastrobin,pyraoxystrobin and fenaminstrobin)in different vegetation types of soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry was developed.The strobilurin fungicides were extracted with 0.1%(volume percentage)acetic acid-acetonitrile,and cleaned-up with 100 mg primary secondary amine(PSA)and 100 mg C 18.The separation was performed on a C 18 column with methanol and water as the mobile phases.The strobilurin fungicides were determined in the positive ion mode and multiple reaction monitoring mode.The quantification was carried out by the matrix-matched external standard curve.The results showed good linear relationships for all analytes in the range of 0.1-100μg/kg with the correlation coefficients of 0.980 5-0.999 9.The mean recoveries of strobilurin fungicides in the spiked soil samples were 65.1%-103.9%and the relative standard deviations were 0.082%-14%(n=3)at three spiked levels(5,10 and 50μg/kg).The limits of quantitation were 0.005-2.0μg/kg.This method is suitable for the trace determination of the 11 strobilurin fungicides in different vegetation types of soil(black soil,red soil,sandy soil,moisture soil,desert grey soil,and plateau soil).