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响应面法在高效液相色谱-二极管阵列检测分析前空气辅助分散液液微萃取大米中脱氧雪腐镰刀菌烯醇的应用及与固相萃取净化的比较。

Application of response surface methodology for air assisted-dispersive liquid- liquid microextraction of deoxynivalenol in rice samples prior to HPLC-DAD analysis and comparison with solid phase extraction cleanup.

机构信息

Department of Chemistry, Faculty of Sciences, University of Sistan and Baluchestan, Zahedan 98135-674, Iran.

Department of Chemistry, Faculty of Sciences, University of Sistan and Baluchestan, Zahedan 98135-674, Iran.

出版信息

Talanta. 2017 Apr 1;165:27-32. doi: 10.1016/j.talanta.2016.12.031. Epub 2016 Dec 16.

Abstract

A fast, simple, and easy to operate air assisted-dispersive liquid-liquid microextraction (AA-DLLME) for preconcentration and extraction of deoxynivalenol (DON) from rice samples is proposed and compared with solid phase extraction (SPE) cleanup. DON was determined using a high performance liquid chromatography with diode-array detection (HPLC-DAD). AA-DLLME was performed using a glass syringe and dispersion of extractant in the sample solution was achieved with help of air bubbles. Chloroform was used as the extractant solvent. To find out the optimized condition for the proposed method, response surface methodology (RSM) was applied for multivariate optimization of effecting parameters namely volume of extractant, number of extraction, pH, and rate of centrifugation. Under optimized condition the dynamic range of calibration graph was found to be 50-500μgL with detection limit of 23.6μgL. Both methods were applied for extraction of DON from rice.

摘要

提出了一种快速、简单、易于操作的空气辅助分散液液微萃取(AA-DLLME)方法,用于从大米样品中预浓缩和提取脱氧雪腐镰刀菌烯醇(DON),并与固相萃取(SPE)净化进行了比较。采用高效液相色谱-二极管阵列检测(HPLC-DAD)法测定 DON。AA-DLLME 使用玻璃注射器进行,通过气泡帮助将萃取剂分散在样品溶液中。氯仿用作萃取溶剂。为了找到该方法的最佳条件,应用响应面法(RSM)对影响参数(萃取剂体积、萃取次数、pH 值和离心速率)进行了多元优化。在优化条件下,校准曲线的动态范围为 50-500μgL,检测限为 23.6μgL。两种方法均用于从大米中提取 DON。

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