固相萃取-气相色谱串联质谱法测定温莪术中19种有机氯和有机磷农药残留

SPE-GC/MS determination of 19 organophosphorus pesticide residues and organochlorine pesticide residues in Rhizoma Curcumae

目的:建立固相萃取-气相色谱串联质谱法测定温莪术中11种有机磷和8种有机氯农药残留,对10种不同批次的温莪术样品进行农药残留测定。方法:温莪术样品用有机溶剂萃取法进行提取,提取溶剂选为乙腈,C18固相萃取小柱净化提取液,用气相色谱-质谱仪分析,采用选择离子模式测定,外标法定量。结果:19种农药成分的峰面积与其质量浓度均有良好的线性关系,相关系数在0.991～1.000。19种农药成分的加标回收率为60.5%～109.3%,RSD为3.9%～10.5%。结论:该方法简便、快速,灵敏度高,重复性好,能够准确地检测温莪术中19种农药残留。

Objective： To establish analytical method for the determination of 11 kinds of organophosphorus pesticide and 8 kinds of organochlorine pesticides in Rhizoma Curcumae by SPE -GC/MS, to quantify the pesticide residues in 10 Rhizoma Curcumae samples. Methods： Rhizoma Curcumas samples were extracted with acetonitrile. The extraction which was purified by SPE column was analyzed by GC - MS. Determination was performed with selected ion monitoring mode and external standard method was adopted in the quantification. Results： 19 kinds of pesticides showed good linearity in a detected concentration range with good correlation coefficient（r =0. 991 -1. 000）. The recoveries of 19 kinds of pesticides were 60. 5% - 109. 3% with RSD of 3.9% - 10. 5%. Conclusion： The method is effective, fast, accurate, repeatable, and can detect 19 kinds of pesticides residues accurately in Rhizoma Curcumae samples.