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机构地区:[1]福建师范大学化学与化工学院,福州350007 [2]福州大学,食品安全分析与检测教育部重点实验室,福州350002
出 处:《分析试验室》2012年第11期33-36,共4页Chinese Journal of Analysis Laboratory
基 金:福建省属高校科研专项基金(JK2010008);福州大学食品安全分析与检测教育部重点实验室开放基金(FS11003);福建师范大学本科生课外科技计划(BKL2010-026);福建省大学生创新性实验计划项目(Fjnu2010-006)资助
摘 要:建立了场增强样品进样–微乳液毛细管电动色谱(microemulsion electrokinetic chromatography,MEEKC)分析6种酞酸酯的方法,对影响富集过程的因素进行了考察。最佳富集条件为:以压力进样先进一段水柱(5.52 kPa×500s),在富集电压为-15 kV下,样品以电动方式进样富集,样品基质为30mmol/L胆酸钠+30.0 mmol/L硼砂(pH 8.5)。与常规MEEKC方法相比,场增强样品进样在线富集技术使6种酞酸酯的检测灵敏度提高了1.6~1000倍,检测限(S/N=3)为1~500 ng/mL。所建立的方法用于食品塑料袋中酞酸酯的测定,加标回收率为92.5%~112.2%。A simple, sensitive, and reproducible method based on field enhanced sample injection (FESI) - microemulsion electrokinetic chromatography (MEEKC) was developed for analysis of six phthalate esters (PAEs). Several factors influencing on-line stacking process were investigated. The optimum stacking conditions were as follows : 30 mmol/L SC + 30. 0 mmol/L borate ( pH 8.5) as sample matrix, - 15 kV as the stacking voltage, 5.52 kPa - 500 s as the amount of water injection. FESI coupled with the MEEKC method increased sensitivity of 1.6 to 1000 fold for six PAEs compared with normal MEEKC. Under the optimum conditions, the detection limits ( S/N = 3) of the six PAEs were in the range of 1.0 - 500. 0 ng/mL. The developed method has been successfully applied to the determination of PAEs in plastic-packaging bags, and the recoveries were from 92. 5 % to 112. 2 % with the intraday relative standard deviation (RSD) less than 6.5 %.
关 键 词:微乳液毛细管电动色谱 场增强样品进样 酞酸酯
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