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一锅法制备丙烯酰化 β-环糊精-硅胶杂化整体柱及其用于测定多菌灵和克百威。

One-pot preparation of an acryloyled β-cyclodextrin-silica hybrid monolithic column and its application for determination of carbendazim and carbaryl.

机构信息

Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules & College of Chemistry and Chemical Engineering, Hubei University, Wuhan 430062, China.

Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Ministry-of-Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules & College of Chemistry and Chemical Engineering, Hubei University, Wuhan 430062, China.

出版信息

Food Chem. 2018 Dec 15;269:181-186. doi: 10.1016/j.foodchem.2018.07.006. Epub 2018 Jul 2.

DOI:10.1016/j.foodchem.2018.07.006
PMID:30100422
Abstract

This work describes, for the first time, an acryloyled β-cyclodextrin hybrid monolith column was synthesized, under aqueous-phase conditions, and used for solid-phase microextraction of carbendazim and carbaryl. The monolithic column was characterized using scanning electron microscopy, nitrogen adsorption-desorption, thermogravimetric analysis and Fourier transform infrared spectroscopy, and used as the adsorbent for solid phase microextraction (SPME) of carbendazim and carbaryl. After optimization of the SPME conditions, a simple and sensitive SPME-HPLC method was developed for the determination of carbendazim and carbaryl in leafy vegetables. The method exhibited a good liner response in the range 5-400 μg/kg (R = 0.9994) for carbendazim and 10-400 μg/kg (R = 0.9996) for carbaryl, respectively. The limits of detection were 1.0 and 1.5 μg/kg for carbendazim and carbaryl, respectively, in leafy vegetables. Recoveries ranged from 92.6% to 110.1%, and the relative standard deviations were less than 6.1%.

摘要

本文首次描述了在水相条件下合成的丙烯酰化 β-环糊精杂化整体柱,并将其用于苯菌灵和克百威的固相微萃取。通过扫描电子显微镜、氮吸附-解吸、热重分析和傅里叶变换红外光谱对整体柱进行了表征,并将其用作苯菌灵和克百威固相微萃取(SPME)的吸附剂。在优化 SPME 条件后,建立了一种简单灵敏的 SPME-HPLC 方法,用于测定叶菜中的苯菌灵和克百威。该方法对苯菌灵的线性响应范围为 5-400μg/kg(R=0.9994),对克百威的线性响应范围为 10-400μg/kg(R=0.9996)。苯菌灵和克百威在叶菜中的检出限分别为 1.0 和 1.5μg/kg。苯菌灵和克百威的回收率在 92.6%至 110.1%之间,相对标准偏差均小于 6.1%。

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