气相色谱-串联质谱法结合QuEChERS法快速检测中药中50种农药残留

Rapid analysis of 50 pesticide residues in traditional Chinese medicine using QuEChERS method and gas chromatography-tandem mass spectrometry

目的 建立运用气相色谱-串联质谱(GC-MS/MS)法快速筛查460份中药材及其中药饮片(43份)中常用的50种农药残留。方法 通过对比《中国药典》2020版中药中农药残留的前处理方法,优选中药中50种农药残留的适配性前处理方法。中药样品经乙腈溶剂提取,以Qu ECh ERS法处理,采用GC-MS/MS测定,内标法定量。结果 在460份检测样品中共检出农药残留66份,总检出率为14.3%,检出禁用农药6份,检出率为1.3%,43份中药饮片中农药残留检出率为11.6%,未检出禁用农药。农残的检出是季节性分布集中出现在第3、4季度,农贸市场和种植地的农残检出率明显高于医院和药店,并且存在农残超标情况。中药中根类和叶类受污染最重,中药材全草类中农药残留最多,检出率为20.4%,其次为叶类18.3%和根茎类16.3%,中药饮片中农残最高为叶类,检出率为15.4%,全草类检出率为11.1%、根茎类检出率为6.2%,全草类、根茎类和叶类存在样品中检出多种农药残留的现象。结论 该方法简单快速、灵敏度高、重现性好、准确度高,可快速筛查中药中农药残留,为保障中药质量提供参考。

Objective To develop a method of gas chromatography-tandem mass spectrometry(GC-MS/MS)to determine 50 pesticide residues in Chinese medicinal materials(460 samples)and decoction pieces(43 samples).Methods A suitable pretreatment method of 50 pesticide residues in medicines was obtained by optimizing and comparing the pretreatment method with Chinese Pharmacopoeia(2020 edition).The pesticide residues in medicines were extracted with acetonitrile,the extraction was pretrested with QuEChERS,then,the target pesticides were detected by GC-MS/MS and quantified by the internal standard method.Results A total of 66 pesticide residues were detected in 460 samples,the total detection rate was 14.3%,the detection rate of banned pesticides was 1.3%.The detection rate of pesticide residues in decoction pieces was 11.6%,no banned pesticides were detected.The detection of pesticide residues was concentrated in the 3rd and 4th quarters with seasonal distribution,the detection rate of pesticide residues in farmers'markets and planting areas was significantly higher than that in hospitals and pharmacies,and there were cases of excessive pesticide residues.The rhizomes and leaves were the most seriously polluted,the pesticide residue rate of whole grass in Chinese medicinal materials was the highest(20.4%),followed by leaves(18.3%)and rhizomes(16.30%).The highest pesticide residue rate of decoction pieces was leaves(15.4%),followed by whole grass(11.1%)and rhizomes(6.2%),and many kinds of pesticide residues were detected in the samples of whole grass,rhizomes and leaves.Conclusion The established method is simple,accurate and selective,and suitable for the rapid determination of multiple pesticide residues in traditional Chinese medicine(TCM),which provides references for ensuring the quality of TCM.