QuEChERS-气相色谱法测定葡萄酒中6种杀虫剂

Determination of 6 insecticides in wine by QuEChERS-gas chromatography

目的建立QuEChERS-气相色谱法测定葡萄酒中6种杀虫剂残留的分析方法。方法样品经乙腈提取后,提取液采用QuEChERS前处理后上机测定。优化的色谱条件为:DB-1石英毛细管柱(0.53 mm×1.50μm,30m),采用程序升温分离,火焰光度检测器检测,采用外标法定量。结果在优化的条件下,6种杀虫剂在0.01~1.50μg/mL范围内线性良好,相关系数(r)均大于0.999,定量限为0.02~0.025 mg/kg, 6种杀虫剂平均回收率为81%~115%,相对标准偏差(relative standard deviation, RSD)在0.870%~7.29%(n=3)之间。结论该方法具有操作简便、快速、准确的特点,适用于葡萄酒中6种杀虫剂残留痕量分析。

Objective To establish a method for the determination of 6 insecticides in wine by gas chromatography combined with QuEChERS. Methods After extracted with acetonitrile, the sample extract was pretreated by QuEChERS method. Under the optimized chromatographic conditions, the analysis was carried out with a capillary column(DB-1, 0.53 mm×1.50 μm, 30 m), monitoring with an flame-photometric detector, the 6 insecticides were separated by temperature-programming of the column. External standard method was used for quantitative analysis. Results Under the optimized conditions, good linearities were obtained in the range of 0.01-1.50 μg/mL for 6 insecticides with the correlation coefficients greater than 0.999 by external method, the limits of quantification of the method were 0.02 mg/kg to 0.025 mg/kg. The average recoveries of the six kinds of insecticide ranged from 81% to 115% with the relative standard deviations(RSDs) from 0.870% to 7.29%. Conclusions The method is simple, rapid and accurate, and can be used for the routine analysis of 6 insecticides residues in wine.