摘要
[目的]建立测定中药材中N-甲基氨基甲酸酯类农药残留量的高效液相色谱-柱后衍生-荧光检测分析方法。[方法]样品经乙腈-水超声提取,经无水硫酸钠-PSA柱吸附净化,用液相色谱法进行定量测定。[结果]6种N-甲基氨基甲酸酯类农药标准曲线线性关系良好,相关系数r为0.996~0.999,检出限为0.01~0.02 mg/kg,在3个加标水平下,6种农药的平均回收率为83.3%~107.5%,相对标准偏差为2.5%~11.3%。[结论]该方法准确、快速、净化效果好,可满足农药残留的检测要求。
[Aims] The aims were to establish a method for determination of N-methyl carbamate pesticide residues in Chinese herbal medicine by HPLC-post column derivatization-fluorescence detection. [Methods] The samples were extracted with acetonitrile-water, purified with anhydrous sodium sulfate-PSA, and quantified by HPLC. [Results] The linear relationship for six kinds of N-methyl carbamate pesticide was good, the correlation coefficient was 0.996-0.999,the limit of detection was 0.01-0.02 mg/kg, the average recoveries of the 6 pesticides at the 3 spiked levels were83.3-107.5%, the relative standard deviation was 2.5-11.3%. [Conclusions] The method is accurate, rapid, and has good purification effect, which can meet the requirements of pesticide residue detection.
引文
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