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中国药物评价 ›› 2021, Vol. 38 ›› Issue (1): 62-69.

• 评价技术与方法 • 上一篇    下一篇

GC-MS/MS方法测定卷柏中66种农药残留

霍甜甜1, 李彦超1, 周宁2, 郑晓珂2   

  1. 1. 河南省食品药品检验所, 国家药品监督管理局中药材及饮片质量控制重点实验室,河南 郑州 450018;
    2. 河南中医药大学,河南 郑州 450046
  • 收稿日期:2020-11-16 修回日期:2020-05-26 出版日期:2021-02-28 发布日期:2021-02-28
  • 基金资助:
    国家重大新药创制-科技重大专项(2013ZX09102-022)

Determination of 66 Kinds of Pesticide Residues in Herba Selaginellae by GC-MS/MS

  1. 1. NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(Chiense Materia Medica and Prepared     Slices),Henan Institute for Food and Drug Control, Henan Zhengzhou 450018, China;
    2. Henan University of Chinese Medicine, Henan Zhengzhou 450046, China
  • Received:2020-11-16 Revised:2020-05-26 Online:2021-02-28 Published:2021-02-28

摘要: 目的:建立同时分析测定卷柏中66种农药残留的GC-MS/MS方法。方法:样品经乙腈提取,采用分散固相萃取净化管净化,氮吹浓缩,定容后过滤。采用GC-MS/MS联用法测定卷柏中的农药残留量。结果:在实验条件下,66种农药组分能很好地分离检测,在相应的测定范围4.8~250 ng·mL-1内线性关系良好,相关系数均大于0.991,各成分的检出限均在0.000 5~0.005 mg·kg-1之间,方法的精密度和重复性RSD均小于5%,加标回收率在69.0%~125.7%之间,RSD均小于10%。结论:该方法灵敏度高,快速简便,可用于对卷柏的农药残留测定。
    

关键词: font-size:medium, ">GC-MS/MS;农药残留;卷柏

Abstract: Objective: To establish a method of 66 pesticide residues in Herba Selaginellae based on GC-MS/MS technique. Methods: Samples were extracted with acetonitrile and purified by the small column of SPA, the analysis was performed by GC-MS/MS. Results: All the 66 pesticides showed good linearities in their reasonable rang(4.8-250 ng·mL-1), R2>0.991, the LODs of each pesticide were all in the range of 0.000 5-0.004 mg·kg-1, the RSD of precision and repeatability of the developed method were less than 5%, and the average recoveries of all the pesticides were in the range of 69.0%-125.7%, the RSD were less than 10%. Conclusion: The method is suitable for the multiresidues analysis of pesticides in Herba Selaginellae owing to its advantages of rapidity, simplicity and better sensitivity.
 

Key words: font-size:medium, ">GC-MS/MS; Pesticide residues; Herba Selaginellae

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