QuEchERs-高效液相色谱柱后衍生法测定茶叶中10种氨基甲酸酯类农药残留

目的:建立了高效液相色谱-柱后衍生法检测茶叶中10种氨基甲酸酯农药残留的方法。方法:氨基甲酸酯农残经过醋酸乙腈(0.1%)快速提取后加入无水硫酸钠、无水硫酸镁,取5 mL提取液经PSA净化,取1 mL净化液用氮气吹干,准确取1 mL乙腈水(1+1)复溶,用高效液相色谱柱后衍生法测定,外标法定量。结果:10种氨基甲酸酯农药在0.01~0.5 μg/mL范围内线性关系良好,相关系数为0.9996~0.9999。检出限为0.01~0.02 mg/kg,平均加标回收率为81.98%~95.59%,相对标准偏差为1.22%~4.98%。结论:本方法准确度高、精密度好、简便、快速,适用于茶叶中氨基甲酸酯农药残留的检测。

Simultaneous Determination of Ten Carbamate Pesticide Residues in Tea by QuEChERS-HPLC with Post-column Derivatization

Objective:To establish a method for detecting ten carbamate pesticide residues in tea by QuEChERS-HPLC with post-column derivatization. Method:The carbamat pesticide residues were extracted with acetic acetonitrile solution(0.1%)followed by adding 1 g anhydrous magnesium sulfate and 1 g anhydrous sodium acetate. After 5 mL extraction processed by PSA powder,1 mL purified solution was concentrated to near dry and dissolved by accurate 1 mL acetonitrile water solution(1+1),then detected by HPLC with post-column derivatization,quantified by external standard method. Result:The ten carbamate pesticide residues had good linearities at the rang of 0.01 to 0.5 μg/mL,the correlation coefficient were 0.9996~0.9999 and the limits of detection were 0.01~0.02 mg/kg. The average recovery rates of ten carbamate pesticide residues in 3 spiked levels ranged from 81.97% to 95.59% with the relative standard deviations(RSDs)were 1.22%~4.98%. Conclusion:The proposed method was accurate,precise,convenient and rapid,which is suitable for the determination of ten carbamate pesticide residues in tea.