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采用动态微波辅助萃取-漂浮有机液滴固化结合高效液相色谱法测定谷物中的三嗪类除草剂。

Determination of triazine herbicides in cereals using dynamic microwave-assisted extraction with solidification of floating organic drop followed by high-performance liquid chromatography.

机构信息

College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China.

出版信息

J Chromatogr A. 2012 Apr 13;1233:36-43. doi: 10.1016/j.chroma.2012.02.034. Epub 2012 Feb 21.

Abstract

A simple and cost-effective method of dynamic microwave-assisted extraction (DMAE) combined with solidification of floating organic drop (SFO) was developed for determining the five triazine herbicides in cereals. The approach combines the advantages of DMAE and SFO technique, and up to 15 samples can be treated simultaneously in 16 min. Firstly, triazine herbicides were extracted with 1 mL of methanol containing 90 μL of 1-dodecanol and following with 10 mL of water under the action of microwave energy. After that, 1.5 g sodium chloride was added into the obtained extract, and the mixture was centrifuged and cooled. The 1-dodecanol drop which contained the target analytes was solidified and transferred for analysis by HPLC-UV. Limits of detection of the five triazines obtained were in the range of 1.1-1.5 ng g(-1). Relative standard deviations of intra- and inter-day tests ranging from 5% to 7% were obtained. The method was successfully applied to the analysis of ten cereals and the recoveries of the triazines for the spiked samples were in the range of 80-102%. The proposed method is an alternative approach to the analysis of triazine herbicides in complex solid samples, being more rapid and simpler compared with the traditional extraction method.

摘要

一种简单且经济高效的动态微波辅助萃取(DMAE)与漂浮有机液滴固化(SFO)相结合的方法,用于测定谷物中的五种三嗪类除草剂。该方法结合了 DMAE 和 SFO 技术的优点,在 16 分钟内可同时处理多达 15 个样品。首先,在微波能量的作用下,用含有 90 μL 1-十二醇的 1 mL 甲醇提取三嗪除草剂,然后用 10 mL 水萃取。之后,向所得提取物中加入 1.5 g 氯化钠,混合液离心并冷却。含有目标分析物的 1-十二醇液滴凝固并转移到 HPLC-UV 进行分析。五种三嗪的检测限在 1.1-1.5 ng g(-1) 范围内。日内和日间测试的相对标准偏差在 5%-7%之间。该方法成功应用于十种谷物的分析,加标样品中三嗪的回收率在 80%-102%范围内。与传统的提取方法相比,该方法更快速、更简单,是分析复杂固体样品中三嗪类除草剂的一种替代方法。

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