QuEChERS/超高效液相色谱-串联质谱法检测果酒中14种甲氧基丙烯酸酯类杀菌剂

Determination of 14 Strobilurin Fungicides Residues in Fruit Wines by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with QuEChERS

利用QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)建立了同时检测果酒中14种甲氧基丙烯酸酯类杀菌剂残留量的分析方法。样品用乙腈提取,经200 mg C_(18)+600 mg无水MgSO_(4)净化,过0.2μm滤膜后上机检测。采用Phenomenex Kinetex F5(3.0 mm×100 mm,2.6μm)色谱柱进行分离,以乙腈-水为流动相进行梯度洗脱,采用电喷雾正离子(ESI+)模式电离,在多反应监测(MRM)模式下进行检测,外标法定量。结果表明:14种甲氧基丙烯酸酯类杀菌剂在各自的质量浓度范围内线性关系良好,相关系数(r^(2))均大于0.999,方法检出限(LOD)和定量下限(LOQ)分别为0.002~0.723μg/kg和0.006~2.409μg/kg。空白样品在5、10、50μg/kg加标水平下的回收率为71.2%~99.1%,相对标准偏差(RSD,n=7)为0.30%~9.4%。该方法操作简便、高效灵敏、准确度好,适用于果酒中甲氧基丙烯酸酯类杀菌剂残留的检测。

A reliable analytical method was developed for the simultaneous determination of 14 strobilurin fungicides in fruit wines based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with QuEChERS.The samples were firstly extracted with acetonitrile,then purified by a modified QuEChERS method(200 mg C18 and 600 mg anhydrous MgSO_(4)),filtered through a 0.2μm microporous membrane,and finally determined using the UPLC-MS/MS system.The seperation was performed on a Phenomenex Kinetex F5(3.0 mm×100 mm,2.6μm)column by gradient elution,with acetonitrile and water as the mobile phases.The strobilurin fungicides were determined in positive electrospray ionization mode under multiple reaction monitoring(MRM)mode,and quantified by external standard method.Results showed that good linear relationships for the analytes existed in their respective ranges,with correlation coefficients(r^(2))all larger than 0.999.The limits of detection(LOD)and the limits of quantitation(LOQ)of the method were in the ranges of 0.002-0.723μg/kg and 0.006-2.409μg/kg,respectively.The recoveries for 14 strobilurin fungicides at three spiked levels of 5,10 and 50μg/kg ranged from 71.2% to 99.1% with relative standard deviations(RSD,n=7)of 0.30%-9.4%.This method is simple,efficient,sensitive and accurate,and could be applied to the determination of strobilurin fungicide residues in fruit wine.