HPLC-MS测定白酒中氨基甲酸酯类农药残留

建立了一种同时对白酒中10种氨基甲酸酯类农药残留的HPLC-MS测定方法。色谱条件:色谱柱Phenomenex-LunaCN100A(250mm×4.6mm×5μm),流动相乙腈-水(在40min内乙腈由20%变为80%),流速1.00mL/min,检测波长195nm,柱温25℃,进样量20μL。质谱条件:电喷雾离子源(ESI+源),扫描范围(m/z)为50～350,干燥气温度350℃,干燥气流速8.0mL/min,雾化气压力275.86kPa。样品制备:白酒样品用固相萃取处理后,氮吹浓缩,乙腈定容至2mL。结果表明,10种氨基甲酸酯类农药残留在0.05～3μg范围积线性关系良好,相关系数R2>0.99。平均回收率在72.6%和97.6%,RSD在2.6%～5.9%之间。结论:方法灵敏度高、操作简便、结果准确,可用于酒样中痕量农药残留的含量测定。

Determination of carbamates pesticides in liquor by HPLC/MS

A HPLC/MS method has been established for the determination of ten carbamates pesticides in liquor.The chromatographic conditions are as follows:Column of Phenomenex-Luna CN 100 A(250 mm×4.6 mm×5 μm),and mobile phase was acetonitrile-water(20:80～80:20 within 40 minutes),flow rate was 1.0 mL/min,wavelength was 195 nm,column temperature was 25 ℃ and the injection volume was 20 μl..MS conditions:Scanning range is 50～350 m/z,temperature of drying gas is 350 ℃,flow rate of drying gas is 8.0 mL/min,pressure of the evaporative gas is 275.86 kPa.The liquor samples were treated by SPE(solid phase extraction,NH2) and then concentrated by nitrogen-blow.Results showed that the standard curves of ten carbamates were linear over the quality range of 0.05～3 μg/mL,the correlation coefficient r were over 0.99.The average recovery of carbamates were 72.6%～97.6%,RSD were 2.6%～5.9%.Conclusion:this method was accurate,rapid,sensitive for the determination of carbamates pesticides in liquor by HPLC/MS.