高效液相色谱串联质谱测定甘蔗中12种氨基甲酸酯类农药残留

Determination of 12 Carbamate Pesticide Residues in Sugarcane by HPLC-MS/MS

建立了甘蔗中12种常用的氨基甲酸酯类农药残留的高效液相色谱串联质谱(HPLC-MS/MS)检测方法。甘蔗样品用乙腈提取,经QuEChERS方法净化后,采用HPLC-MS/MS进行分析检测,在多反应监测模式(MRM)下,外标法定量,线性良好(r2>0.995),检出限为0.03～0.19μg/kg。分别在样品中添加标准农药样品10、50、100μg/kg水平上进行添加回收率实验,方法的回收率范围为81.3%～108.1%,相对标准偏差为0.8%～4.7%(n=6)。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,满足甘蔗中氨基甲酸酯类农药残留检测要求。

A method was developed for the determination of 12 carbamate pesticide residues in sugarcane by high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS）. The residues in the samples were extracted by acetonitrile, cleaned up by developed QuEChERS method, and then analyzed by using HPLC-MS/MS in multiple reaction monitoring （MRM） mode via positive electrospray ionization. External standard method was used to determine the residue contents with a good linear relationship （r^2〉0.995）. The limits of quantification （LOQ） were 0.03-0.19 μg/kg. The recoveries of carbamate pesticide residues at three levels of 10, 50, and 100 μg/kg were from 81.3% to 108.1% with the relative standard deviations （RSDs） of 0.8%-4.7% （n=6） in sugarcane. The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis. This developed procedure is suitable for the determination of carbamate pesticide residues in sugarcane.