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蔬菜中气固萃取用气动雾化对三嗪类除草剂的研究。

Pneumatic nebulization gas-solid extraction of triazine herbicides in vegetable.

机构信息

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

出版信息

J Chromatogr A. 2013 Aug 23;1304:18-27. doi: 10.1016/j.chroma.2013.06.061. Epub 2013 Jun 29.

Abstract

The pneumatic nebulization gas-solid extraction (PN-GSE) high-performance liquid chromatography (HPLC) was developed and applied to the extraction, separation and determination of triazine herbicides in vegetables. The herbicides were ultrasonically extracted from vegetables with 70% methanol in water. Then the extract was introduced to PN-GSE system to further clean-up. The experimental parameters, including type and concentration of extraction solvent, ratio of solvent to sample, pH value of sample solution and PN-GSE solution, extraction time, temperature, type of sorbent, flow rate of carrier gas, pumping rate of gas, and kind and volume of elution solvent, were investigated and optimized. The limits of detection for seven herbicides range from 0.59 to 1.05μg/kg. The recoveries of the herbicides are in the range of 86.2-110.6% and relative standard deviations are equal or less than 7.51%, when the present method was applied to the analysis of spiked samples. The present method was applied to the analysis of real samples and the results were satisfactory.

摘要

气动雾化气固萃取(PN-GSE)高效液相色谱法(HPLC)被开发并应用于蔬菜中三嗪类除草剂的提取、分离和测定。除草剂通过水的 70%甲醇超声提取自蔬菜。然后,将提取物引入 PN-GSE 系统进行进一步的净化。实验参数,包括萃取溶剂的类型和浓度、溶剂与样品的比例、样品溶液和 PN-GSE 溶液的 pH 值、萃取时间、温度、吸附剂的类型、载气的流速、气体的抽提率以及洗脱溶剂的种类和体积,进行了考察和优化。七种除草剂的检测限范围为 0.59 至 1.05μg/kg。当本方法应用于加标样品的分析时,除草剂的回收率在 86.2-110.6%之间,相对标准偏差等于或小于 7.51%。本方法应用于实际样品的分析,结果令人满意。

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