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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。
A simultaneous HPLC-MS method was developed for the determination of 10 carbamate pesticide residues in white spirit. Chromatographic conditions: column Phenomenex-LunaCN100A (250 mm × 4.6 mm × 5 μm), mobile phase acetonitrile-water (acetonitrile from 20% to 80% in 40 min), flow rate 1.00 mL / min, , Injection volume 20μL. Mass spectrometry conditions: electrospray ionization source (ESI + source) with scanning range (m / z) of 50-350, drying temperature of 350 ℃, drying gas flow rate of 8.0 mL / min and atomizing gas pressure of 275.86 kPa. Sample Preparation: Liquor samples were extracted by solid-phase extraction and concentrated by nitrogen. The volume of acetonitrile was fixed to 2 mL. The results showed that the linear relationship of 10 carbamate pesticide residues in the range of 0.05 ~ 3μg was good with the correlation coefficient R2> 0.99. The average recoveries were 72.6% and 97.6% with RSDs between 2.6% and 5.9%. Conclusion: The method has high sensitivity, simple operation and accurate results. It can be used for the determination of trace pesticide residues in wine samples.