高效液相色谱-串联质谱法测定粮谷中9种氨基甲酸酯类农药残留

本研究采用了高效液相色谱-串联质谱联用(HPLC-MS/MS)技术,建立了高灵敏度的同时检测粮谷中9种氨基甲酸酯类农药残留量的方法。样品经乙腈提取,中性氧化铝填充柱净化,然后采用HPLC-ESI( )-MS/MS测定。对液-质分离条件和样品前处理条件进行了优化。9种氨基甲酸酯类农药在0.1~100μg/L范围内线性良好,相关系数为0.9986~0.9998。在0.001~0.05mg/kg浓度范围内,平均加标回收率在73.40%~102.01%之间;相对标准偏差为1.25%~9.94%。该方法简便、快速、灵敏、净化效果好。可同时满足进、出口粮谷中多种氨基甲酸酯类农药残留量的检验工作需要。

Simultaneous Determination of Carbamate Pesticide Residues in Grains By High Performance Liquid Chromatography Tandem Mass Spectrometry

A high performance liquid chromatography/electrospray ionization tandem mass spectrometric method has been developed for the simultaneous determination of nine carbamate pesticide residues in grains. Carbamate pesticides were extracted with acetonitrile, cleaned up with neutral-alumina column, and then analyzed by high performance liquid chromatography-electrospray(HPLC-ESI)(+)-tandem mass spectrometry(MS/MS). Sample pre-treatment and LC-MS/MS analytical conditions were optimized. The linear range was 0.1-100 g/L, the correlation coefficients were 0.9986-0.9998. The average recoveries of nine carbamate pesticides in spiked grains (from 0.001 to 0.05 mg/Kg) ranged from 73.40% to 102.0%, and the relative standard deviation were between 1.3% and 9.9%. The results indicate that the method developed is easier, faster, more sensitive and has a better purification effect. It also demonstrats that this multiresidue analysis method can meet the requirements for simultaneous determination of many carbamate pesticides in grains for import & export inspection.