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目的建立分散固相萃取气相色谱法测定山茱萸中有机氯和拟除虫菊酯类农药残留的方法。方法选用乙腈为提取溶剂,丙基乙二胺(PSA)为分散净化剂;采用Hp-5毛细管气相色谱柱分离,电子捕获检测器进行检测。结果有机氯和拟除虫菊酯分别在5~500μg.L-1和10~1 000μg.L-1内呈良好线性关系,相关系数均大于0.997 8;检定量限为1~5μg.L-1;平均回收率为78.32%~112.80%,RSD为3.2%~9.4%。结论本方法适用于中药材中的农药多残留的测定与安全监控。
Objective To establish a method for the determination of organochlorine and pyrethroid pesticide residues in Fructus Corni by dispersive solid phase extraction and gas chromatography. Methods Acetonitrile was used as extraction solvent and propylethylenediamine (PSA) was used as dispersant. Hp-5 capillary gas chromatographic column was used for separation and electron capture detector was used for detection. Results The results showed that there was a good linear relationship between organochlorine and pyrethroid in the range of 5 ~ 500μg.L-1 and 10 ~ 1 000μg.L-1, respectively. The correlation coefficients were all greater than 0.997 8. The limits of detection were 1 ~ 5μg.L-1. The average recovery was 78.32% ~ 112.80%, RSD was 3.2% ~ 9.4%. Conclusion This method is suitable for the determination and safety monitoring of pesticide residues in Chinese herbal medicines.