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Analysis of pesticide residues in commercially available chenpi using a modified QuEChERS method and GC-MS/MS determination.
Journal of Pharmaceutical Analysis ( IF 6.1 ) Pub Date : 2019-01-31 , DOI: 10.1016/j.jpha.2019.01.005
Shuang Li 1, 2 , Peipei Yu 1 , Ceng Zhou 1 , Ling Tong 3 , Dongxiang Li 3 , Zhiguo Yu 1 , Yunli Zhao 1
Affiliation  

To ensure the safety of the commercially available chenpi, a convenient and fast analytical method was developed for the determination of 133 pesticide residues in chenpi using gas chromatography-tandem mass spectrometry (GC-MS/MS). In this study, different extraction solvents, redissolution solvents and adsorbents were tested according to the recovery and purification effect to obtain a modified QuEChERS method. The samples were extracted with acetonitrile. During the clean-up step, octadecyl-modified silica (C18) and graphitized carbon black (GCB) were selected, and aminopropyl (NH2) was used instead of primary secondary amine (PSA) because of its weaker ion exchange capacity which had little effect on the recovery of ditalimfos. Samples were quantified by matrix-matched calibration with internal standards. All pesticides showed good linearity in the respective range, both with values of r2 > 0.99. The average recoveries of the pesticides spiked samples ranged from 70.0% to 112.2% with the RSDs of 0.2%–14.4%. The modified QuEChERS method was validated and applied to twenty real samples. Five pesticides were found in eight batches, but no pesticide exceeded the maximum residue limits (MRL, MRL reference to European commission).



中文翻译:

使用改良的QuEChERS方法和GC-MS / MS测定方法可对商用chenpi中的农药残留进行分析。

为确保市售chenpi的安全性,开发了一种便捷,快速的分析方法,使用气相色谱-串联质谱(GC-MS / MS)测定chenpi中的133种农药残留。在这项研究中,根据回收和纯化效果测试了不同的萃取溶剂,再溶解溶剂和吸附剂,从而获得了改良的QuEChERS方法。样品用乙腈萃取。在清除步​​骤中,选择了十八烷基改性的二氧化硅(C18)和石墨化的炭黑(GCB),以及氨丙基(NH 2用)代替伯仲胺(PSA),因为它的离子交换能力较弱,对双talimfos的回收几乎没有影响。通过与内标物进行基质匹配的校准对样品进行定量。所有农药在各自的范围内均表现出良好的线性,r 2 > 0.99。加标农药的平均回收率在70.0%至112.2%之间,相对标准偏差(RSD)为0.2%至14.4%。改进的QuEChERS方法得到验证,并应用于二十个真实样本。在八批次中发现了五种农药,但没有农药超过最大残留限量(MRL,MRL参考欧洲委员会)。

更新日期:2019-01-31
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