首页> 外文期刊>Journal of separation science. >Analysis of kresoxim-methyl and its thermolabile metabolites in Korean plum: An application of pepper leaf matrix as a protectant for GC amenable metabolites
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Analysis of kresoxim-methyl and its thermolabile metabolites in Korean plum: An application of pepper leaf matrix as a protectant for GC amenable metabolites

机译:红李中克雷索辛甲基及其热不稳定代谢产物的分析:辣椒叶基质作为GC适宜代谢产物的保护剂的应用

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摘要

A new method was developed for kresoxim-methyl (parent compound) and its two thermolabile metabolites, BF 490-2 and BF 490-9, in Korean plum, introducing pepper leaf matrix as a natural analyte protectant for GC-amenable metabolites using a GC-electron capture detector. Samples were extracted with a simple and rapid method using a mixture of ethyl acetate–n-hexane (1:1) and salts, and purified via SPE. Due to the elution gap between parent compound and metabolites in the SPE cartridge and matrix interference, kresoximmethyl was isolated separately from its metabolites. An optimized amount of pepper leaf matrix (0.25 g/mL) was added to the metabolites prior to each injection. Calibration curves were linear over the concentration ranges with coefficient of determination (r~2) ≥ 0.999. The method was validated in triplicate at two fortification levels, giving recoveries ranging between 74.3 and 101.4%, and RSDs less than 5%. The LOD and LOQ were 0.015 and 0.05 mg/kg, respectively. The method was successfully applied to real samples where kresoxim-methyl residues were detected in field-incurred plum samples. Residues were confirmed using GC-MS.
机译:开发了一种新方法用于克雷索辛甲基(母体化合物)及其两种对热不稳定的代谢产物BF 490-2和BF 490-9,在朝鲜李中引入了胡椒叶基质作为使用GC的适合GC代谢物的天然分析物保护剂-电子捕获检测器。使用乙酸乙酯-正己烷(1:1)和盐的混合物,以简单,快速的方法提取样品,然后通过SPE纯化。由于SPE小柱中母体化合物与代谢物之间的洗脱间隙以及基质干扰,因此将kresoximimmethyl与代谢物分开分离。在每次注射前,将最适量的胡椒叶基质(0.25 g / mL)添加到代谢物中。校准曲线在浓度范围内是线性的,测定系数(r〜2)≥0.999。该方法在两个设防水平上一式三份进行了验证,回收率在74.3%至101.4%之间,RSD小于5%。 LOD和LOQ分别为0.015和0.05 mg / kg。该方法已成功应用于在野外梅子样品中检测到克雷索辛甲基残留的实际样品中。使用GC-MS确认残留物。

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