MPFC-QuECHERS结合超高效液相色谱串联质谱法快速测定铁皮石斛中56种农药残留

Rapid determination of 56 pesticide residues in Dendrobium officinale by MPFC-QuEChERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry

目的:对铁皮石斛的农药残留量进行风险分析与评估。方法:建立了超滤型净化分散固相萃取(MPFC-QuEChERS)结合超高效液相色谱—串联质谱法快速测定铁皮石斛中56种农药残留的分析方法。样品经0.1%甲酸—乙腈溶液提取,QuEChERS盐析包分层,经超滤净化柱单步净化,采用电喷雾正负离子切换(ESI),动态多反应监测(DMRM)模式进行分析,基质外标法定量。结果:56种农药残留在1.0~250.0μg/L线性范围内线性关系良好(R^(2)>0.99)。方法的检出限(LOD)为1~5μg/kg,定量限(LOQ)为3.0~15.0μg/kg。56种农药残留在各自定量限1,2,10倍加标水平下,平均回收率为75.1%~107.0%,相对标准偏差(RSD)为2.7%~18.9%。采用该方法对20批次铁皮石斛中农药残留进行检测,结果显示,5份样品中检出烯酰吗啉、嘧菌酯、腈苯唑、丙环唑、苯醚甲环唑、啶氧菌酯6种农药,含量范围在0.0667~1.872 mg/kg。结论:超滤型净化QuEChERS结合超高效液相色谱—串联质谱法测定农药残留具有前处理简单、快速高效等优特点,可用于铁皮石斛中多种农药残留快速筛查和分析。

Objective:In order to analyze the risk of pesticide residues in D.officinale,a method for rapid determination of 56 pesticide residues in D.officinale by a kind of ultrafiltration purification column(MPFC-QuEChERS)combined with ultra-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was developed.Methods:The samples were extracted with acetonitrile contained 0.1%formic acid,salted out,shaken,centrifuged,and single-step purified by a MPFC-QuEChERS purification column.Mass spectrometer was operated in the positive and negative ion mode using select reaction monitoring for qualitative and quantitative analysis.Results:The result showed that,the 56 kinds of pesticides showed good linearity when they were in 1.0~250.0μg/L(R^(2)>0.99).The limits of detection(LOD)was 1~5μg/kg.Three levels of 1,2 and 10 times of LOQ were added to the sample,the average recovery of each substance in D.officinale was 75.1%to 107.0%,of which the RSDs were 2.7%~18.9%.Conclusion:This method was used to detect pesticide residues in 20 batches of D.officinale.The results showed that 6 kinds of pesticides were detected in 5 samples with the contents ranging from 0.0667 mg/kg to 1.872 mg/kg.The method is simple,fast and efficient,and could be used for rapid screening and analysis of pesticide residues in D.officinale.