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A Novel Method for the Determination of Fungicide Residues in Tobacco by Ultra-performance Liquid Chromatography–Tandem Mass Spectrometry Combined with Pass-Through Solid-Phase Extraction
Chromatographia ( IF 1.2 ) Pub Date : 2021-06-06 , DOI: 10.1007/s10337-021-04056-5
Wei Xiong , Hao Jing , Demin Guo , Ying Wang , Fei Yang

A novel method for the rapid simultaneous determination of multiple fungicide residues in tobacco was established using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) combined with pass-through solid-phase extraction. After a simple vortex extraction of the samples with acetonitrile, the effective pass-through cleanup procedure was adopted to ensure high extraction efficiency and good sample cleanup. Fungicides were well separated on an ACQUITY UPLC™ BEH C18 column in 10 min by gradient elution with positive mode electrospray ionization tandem mass spectrometry. The analytical performance was demonstrated by the analysis of extracts from tobacco, spiked at three concentration levels ranging from 0.1 to 5.0 mg kg−1 for each pesticide. The recoveries for all compounds were 82.1–104.4% with relative standard deviations (RSDs) less than 10.0%. Good linear relation (r ≥ 0.9986) was achieved for all studied analytes. The LODs for all analytes ranged from 0.84 to 5.81 μg kg−1 and the LOQs ranged from 2.66 to 18.32 μg kg−1, respectively. Twenty actual samples were determined with this method, and all samples were found to have fungicides. Being simple, accurate, and reliable, this method can be used for the determination of multiple fungicide residues in tobacco.



中文翻译:

超高效液相色谱-串联质谱结合直通固相萃取测定烟草中杀菌剂残留的新方法

采用超高效液相色谱-串联质谱 (UPLC-MS/MS) 结合直通固相萃取技术,建立了一种快速同时测定烟草中多种杀菌剂残留的新方法。样品用乙腈进行简单的涡流萃取后,采用有效的直通净化程序,以确保高萃取效率和良好的样品净化效果。杀菌剂在 ACQUITY UPLC™ BEH C18 柱上通过梯度洗脱和正模式电喷雾串联质谱法在 10 分钟内得到很好的分离。对烟草提取物的分析证明了分析性能,在 0.1 到 5.0 mg kg -1 的三个浓度水平下加标每种农药。所有化合物的回收率为 82.1–104.4%,相对标准偏差 (RSD) 小于 10.0%。 所有研究的分析物都实现了良好的线性关系 ( r ≥ 0.9986)。所有分析物的 LOD 范围分别为 0.84 至 5.81 μg kg -1和 LOQ 范围分别为 2.66 至 18.32 μg kg -1。用该方法测定了20个实际样品,发现所有样品都含有杀菌剂。该方法简便、准确、可靠,可用于烟草中多种杀菌剂残留的测定。

更新日期:2021-06-07
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