UPLC-MS/MS测定葡萄酒中3种双酰胺类杀虫剂

建立了葡萄酒中氰虫酰胺、氯虫苯甲酰胺、氟苯虫酰胺等3种双酰胺类杀虫剂残留量的超高效液相色谱-串联质谱(UPLC- MS/MS)检测方法。葡萄酒中的3种双酰胺类杀虫剂经乙腈提取后，用GCB/NH2固相萃取柱净化，以乙腈-5 mmol/L乙酸铵-甲酸作为流动相，梯度洗脱，通过UPLC-MS/MS进行测定。结果表明，3种双酰胺类杀虫剂在质量浓度1～20 μg/L范围内呈良好的线性关系，相关系数(R)≥0.999 5，方法检出限＜1.0 μg/kg；以1.0 μg/kg、2.0 μg/kg、10 μg/kg为添加水平，平均回收率在76.3%～91.1%之间，相对标准偏差(RSD)为3.9%～9.8%。表明该方法快速简便、净化效果好、准确度较好、精密度较高，可应用于葡萄酒中3种双酰胺类杀虫剂的同时测定。

Determination of three kinds of diamides insecticides in wine by UPLC-MS/MS

The detection method of three kinds of diamides insecticides (including cyantraniliprole, chlorantraniliprole, flubendiamide in wine) residual amount in wine was established by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The three kinds of diamides insecticides in wine was extracted by acetonitrile, and the extracting solution was purified by GCB/NH2 solid-phase extraction column, with acetonitrile-5 mmol/L ammonium acetate-methanoic acid as mobile phase, then determined by UPLC-MS/MS after gradient elute. The results showed that three kinds of diamides insecticides had a good linear relationship in the range of 1.2-12.0 μg/ml (R≥0.999 5). The limit of detection of method was less than 1.0 μg/kg. With 1.0 μg/kg, 2.0 μg/kg and 10 μg/kg as adding level, the average recovery rate was 76.3%-91.1%. The relative standard deviation (RSD) was 3.9%-9.8%, which indicated that the method was fast, simple, good purifying effect, good accuracy and high precision, could be applied to the simultaneous determination of three kinds of diamides insecticides in wine.