超高效液相色谱-串联质谱法检测半夏不同炮制品中农药残留

基于超高效液相色谱-串联质谱 (UPLC-MS/MS) 检测技术,建立了半夏炮制品中79种禁用及常用农药多残留的检测方法,并采用该方法对采集的217批样品 (包括法半夏、姜半夏和清半夏) 进行测定。半夏样品经乙腈提取后,以PSA净化,采用UPLC-MS/MS在多反应监测模式 (MRM) 下进行检测。检测结果通过统计软件进行分析,比较半夏不同炮制品间的差异。结果表明:在1~100 μg/L范围内,79种农药的质量浓度与其相应的峰面积间呈现良好的线性关系,决定系数 (R2) 均大于0.99。在3个添加水平 (5 × LOD、10 × LOD和20 × LOD) 下,添加回收率在70%~120%内的农药数量占总数的81.0%,相对标准偏差均小于15% (n = 6)。79种农药的定量限为0.0001~0.1 mg/kg。217批半夏样品中检出农药27种。统计分析发现,多菌灵和克百威的检出结果在法半夏与姜半夏、法半夏与清半夏间存在显著性差异。本研究所建立的农药多残留测定方法指标针对性较强,操作简单,方法灵敏度高,准确性好。

Determination of pesticide residues in Pinelliae Rhizoma processed products by ultra performance liquid chromatography-tandem mass spectrometry

A multi-residue analysis method was developed for the determination of 79 pesticides in Pinelliae Rhizoma processed products using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). This method was applied in the screening of 217 batches (including Pinelliae Rhizoma Praeparatum(PRP), Pinelliae Rhizoma Praeparatum cum Zingibere et Alumine(PRZ) and Pinelliae Rhizoma Praeparatum cum Alumine(PRA)). The samples were extracted with acetonitrile and cleaned up by PSA. Then they were detected by UPLC-MS/MS with multiple reactions monitoring (MRM) mode. Detection results were analyzed by statistical software and the differences among processed products were compared. The results showed that all the pesticides had good linearity when the concentrations varied from 1 to 100 μg/L with the coefficient of determination (R2) higher than 0.99. More than 81.0% of the tested pesticides had recovery rates between 70% to 120% with the RSDs less than 15% (n = 6) under the three spiked levels (5 × limits of detection (LOD), 10 × LOD and 20 × LOD). The limits of quantitative (LOQs) of this method ranged from 0.0001 to 0.1 mg/kg. 27 pesticide residues were detected in 217 batches of samples. Statistical analysis showed that the detection results of carbendazim and carbofuran were significantly different between PRP and PRZ, PRP and PRA. This method was proven to be simple, rapid, sensitive, accurate and suitable for the determination of pesticide residues in Pinelliae Rhizoma.