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

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。

Abstract 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.

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