Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian, PR China.
J Sep Sci. 2010 Dec;33(23-24):3717-25. doi: 10.1002/jssc.201000520.
A novel method using microemulsion electrokinetic chromatography combining accelerated solvent extraction was developed for quantitative analysis of six phthalate esters (PAEs) including dimethyl phthalate, diethyl phthalate, dibutyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, as well as dioctyl phthalate. The effect of each individual component within the microemulsions, i.e. oil phase, surfactant and co-surfactant on resolution of the analytes was systematically studied. Baseline separation of six PAEs was achieved within 26 min by using the microemulsion buffer containing a 60 mmol/L borate buffer at pH 9.0, 0.5% v/v n-octane as oil droplets, 100 mmol/L sodium cholate as surfactant and 5.0% v/v 1-butanol as co-surfactant. The purposed accelerated solvent extraction-microemulsion electrokinetic chromatography method was successfully applied to the determination of trace amount of PAEs in soil samples collected from three different fields in areas of Fujian Province and the contents of dimethyl phthalate, diethyl phthalate, dibutyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate and dioctyl phthalate were 0.63-0.68, 0.32-0.63, 2.53-3.96, 0-1.75, 7.32-11.7 and 0-3.46mg/kg, respectively. It was validated that the results were consistent with those obtained by GC-MS method.
建立了一种利用微乳液电动色谱结合加速溶剂萃取的新方法,用于定量分析六种邻苯二甲酸酯(PAEs),包括邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯。系统研究了微乳液中的各个成分,即油相、表面活性剂和助表面活性剂对分析物分离度的影响。通过使用含有 60mmol/L 硼酸缓冲液(pH 9.0)、0.5%v/v 正辛烷作为油滴、100mmol/L 胆酸钠作为表面活性剂和 5.0%v/v 1-丁醇作为助表面活性剂的微乳液缓冲液,在 26min 内实现了六种 PAEs 的基线分离。所提出的加速溶剂萃取-微乳液电动色谱法成功应用于测定从福建省三个不同地区采集的土壤样品中痕量邻苯二甲酸酯的含量,邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯的含量分别为 0.63-0.68、0.32-0.63、2.53-3.96、0-1.75、7.32-11.7 和 0-3.46mg/kg。验证结果与 GC-MS 方法一致。