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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 method of field enhanced sample injection - microemulsion electrokinetic chromatography (MEEKC) for analyzing six kinds of phthalates was established, and the factors affecting the enrichment process were investigated. The optimal enrichment conditions were as follows: injection of advanced water column (5.52 kPa × 500s) under pressure, enrichment of samples by electric mode at the concentration of -15 kV, the sample matrix was 30 mmol / L sodium cholate + 30.0 mmol / L borax (pH 8.5). Compared with the conventional MEEKC method, the field-enhanced sample injection on-line enrichment technology increased the detection sensitivity of six phthalates by 1.6-1000 times and the detection limit (S / N = 3) was 1-500 ng / mL. The established method was applied to the determination of phthalate esters in food plastic bags. The recoveries were 92.5% ~ 112.2%.