用于通过高效液相色谱法测定牛奶中三嗪类除草剂的双水相萃取法。
Aqueous two-phase extraction for determination of triazine herbicides in milk by high-performance liquid chromatography.
作者信息
Yang Xiao, Yu Rui, Zhang Shaohua, Cao Bocheng, Liu Zhongling, Lei Lei, Li Na, Wang Zhibing, Zhang Liyuan, Zhang Hanqi, Chen Yanhua
机构信息
College of Chemistry, Jilin University, Qianjin Street 2699, Changchun 130012, PR China.
Department of Rehabilitation, the General Hospital of FAW (the Fourth Hospital of Jilin University), Haoyue Road 3788, Changchun 130011, PR China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Dec 1;972:111-6. doi: 10.1016/j.jchromb.2014.10.001. Epub 2014 Oct 8.
A simple extraction method based on acetonitrile-K2HPO4 aqueous two-phase system was developed for separation and enrichment of five triazines in milk samples. Acetonitrile was used for extraction of analytes from milk sample and precipitation of milk protein. Deproteinization and extraction were achieved in one single step. Analytes were extracted into the upper phase of the aqueous two-phase system. The parameters affecting the extraction efficiency, such as the volume of acetonitrile, the type and amount of salts, pH value of sample and extraction time were investigated. The limits of detection of atraton, desmetryn, atrazine, terbumeton and terbuthylazine were 2.1, 2.6, 2.3, 2.8 and 2.5μg/L, respectively. When the present method was applied to the analysis of real milk samples, the recoveries of analytes ranged from 86.3 to 120.6% and relative standard deviations were lower than 7.9%.
建立了一种基于乙腈 - K2HPO4 双水相体系的简单萃取方法，用于牛奶样品中 5 种三嗪类化合物的分离和富集。乙腈用于从牛奶样品中萃取分析物并沉淀牛奶蛋白。一步实现了脱蛋白和萃取。分析物被萃取到双水相体系的上相中。研究了影响萃取效率的参数，如乙腈体积、盐的种类和用量、样品的 pH 值以及萃取时间。莠去通、异戊乙净、莠去津、特丁通和特丁津的检测限分别为 2.1、2.6、2.3、2.8 和 2.5 μg/L。将本方法应用于实际牛奶样品分析时，分析物的回收率在 86.3%至 120.6%之间，相对标准偏差低于 7.9%。
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