高效液相色谱法测定蔬菜中19种氨基甲酸酯类农药的残留量

HPLC Determination of Residual Amounts of 19 Carbamate Pesticides in Vegetables

均质后的蔬菜样品用乙腈提取,SPE-NH2固相萃取小柱净化,采用高效液相色谱法测定净化液中19种氨基甲酸酯类农药的残留量。以PICKERING Carbamate Analysis-C8色谱柱为分离柱,用甲醇和水以不同比例混合的溶液为流动相进行梯度洗脱,在线柱后衍生后,用荧光检测器进行测定。抗蚜威的激发波长为339nm,发射波长为392nm,其余18种氨基甲酸酯类农药的激发波长339nm,发射波长为445nm。19种氨基甲酸酯类农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.002~0.014mg·kg^-1。以空白花菜样品为基体进行加标回收试验,所得回收率为47.7%~110%,测定值的相对标准偏差(n=6)为1.0%~12%。

After homogenization,the vegetable sample was extracted with acetonitrile.SPE-NH2 solid phase extraction column was used for purification.HPLC was applied to the determination of residual amounts of 19 carbamate pesticides in the purified liquid.PICKERING Carbamate Analysis-C8 chromatographic column was used as separated column with mixtures of methanol and water with different mixing ratios as mobile phase in the gradient elution,and fluorescemce detector was used for determination after post column derivation.Excitation wavelength and emission wavelength of pirimicarb were set at 339,392 nm,respectively.Excitation wavelength and emission wavelength of the other 18 carbamate pesticides were set at 339,445 nm,respectively.Linear relationships between values of peak area and mass concentration of the 19 carbamate pesticides were kept in definite ranges,with detection limits(3 S/N)in the range of 0.002-0.014 mg·kg^-1.On the base of blank cauliflower sample,test for recovery was made by standard addition method;values of recovery found were in the range of 47.7%-110%,with RSDs(n=6)of determined values in the range of 1.0%-12%.