液相色谱-串联质谱法同时测定葡萄酒中6种吡唑类杀菌剂

Simultaneous Determination of Six Pyrazole Fungicides in Grape Wine by Liquid Chromatography- Tandem Mass Spectrometry

采用液相色谱-串联质谱建立了同时测定葡萄酒中戊苯吡菌胺、氟唑菌酰胺、吡唑萘菌胺、吡咪唑、联苯吡菌胺、呋吡菌胺6种吡唑类杀菌剂的分析方法。样品用超纯水稀释混匀,经HLB固相萃取柱净化后,采用Agilent ZOBRAX C18色谱柱（2.1 mm×150 mm,5μm）分离;以0.1%乙酸水溶液-乙腈为流动相进行梯度洗脱,目标分析物在多反应监测（MRM）模式下进行定性分析,外标法定量。在优化实验条件下,6种吡唑类杀菌剂在1.0~50.0μg·L-1范围内呈良好的线性关系,相关系数（r2）均不低于0.999 3,方法定量下限为0.1~0.4μg·kg-1。在低、中、高3个加标水平下的平均回收率为72.8%~92.6%,相对标准偏差（RSD）不大于6.7%。该方法简便快速、灵敏度高,可用于葡萄酒中吡唑类杀菌剂的测定。

A liquid chromatography- tandem mass spectrometric（ LC- MS / MS） method was developed for the simultaneous determination of six pyrazole fungicides, including penflufen, fluxapyroxad,isopyrazam,furametpyr,bixafen and rabenzazole in grape wine samples. The sample was diluted with ultrapure water,and then cleaned up by HLB solid phase extraction. The separation was performed on an Agilent ZOBRAX C18column（ 2. 1 mm × 150 mm,5 μm） using a gradient elution program with a mobile phase of 0. 1% acetic acid- acetonitrile. The analyte was determined by electrospray ionization tandem mass spectrometry in multiple reaction monitoring（ MRM） mode,and quantified by the external standard method. The results indicated that the calibration curves for pyrazole fungicides were linear（ r2≥0. 999 3） in the range of 1. 0- 50. 0 μg·L- 1. The limits of quantitation（ LOQs） were in the range of 0. 1- 0. 4 μg·kg- 1. The average recoveries at three spiked levels ranged from 72. 8% to 92. 6% with RSDs not more than 6. 7%. This method is simple,rapid and sensitive,and is suitable for the analysis of six pyrazole fungicides in grape wines sample.