China National Tobacco Quality Supervision and Test Center, Zhengzhou 450001, China.
China tobacco Guizhou Industrial Co. Ltd, Guiyang 550009, China.
J Chromatogr A. 2021 Apr 12;1642:462040. doi: 10.1016/j.chroma.2021.462040. Epub 2021 Mar 5.
This work presents a simple, rapid and green chiral analysis method for five triazole fungicides (penconazole, tebuconazole, triadimefon, myclobutanil, and triadimenol) in tobacco, by which the samples were cleaned up by the novel pass-through solid phase extraction and subsequently the stereoisomers were separated and determined by the supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS). Optimized separation of the stereoisomers was achieved on an ACQUITY UPC2 Trefoil AMY 1 column within 6 min. Under fortified concentration levels of 0.1, 0.5 and 2.0 mg/kg, the mean recoveries were 82.8-106.6%, the intra-day relative standard deviations (RSDs) were 1.1-6.6%, and the inter-day RSDs were 2.5-5.6%. The correlation coefficient was greater than 0.9926 for all studied analytes within the range of 10-500 ng/mL. The limits of detection (LODs) for all stereoisomers ranged from 0.26 μg/kg to 3.24 μg/kg. The established method was subsequently successfully applied to analyze authentic samples, confirming that this method is a novel, rapid and environmentally friendly method for the stereoselective separation of triazole fungicides in tobacco.
本工作建立了一种简单、快速、绿色的手性分析方法，用于烟草中五种三唑类杀菌剂（戊唑醇、丙环唑、三唑酮、腈菌唑和三唑醇）的分析，采用新型穿透固相萃取法对样品进行净化，然后用超临界流体色谱-串联质谱（SFC-MS/MS）对手性异构体进行分离和测定。在手性柱 ACQUITY UPC2 Trefoil AMY 1 上，优化了 6 分钟内的异构体分离。在 0.1、0.5 和 2.0 mg/kg 的加标浓度水平下，平均回收率为 82.8-106.6%，日内相对标准偏差（RSD）为 1.1-6.6%，日间 RSD 为 2.5-5.6%。在所研究的浓度范围内，所有分析物的相关系数均大于 0.9926。所有手性异构体的检测限（LOD）范围为 0.26-3.24μg/kg。该方法随后成功应用于真实样品的分析，证实了该方法是一种新颖、快速、环保的烟草中三唑类杀菌剂立体选择性分离方法。
