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建立了高效毛细管电泳(HPCE)同时测定饮料中苯甲酸、山梨酸、脱氢乙酸和对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯的方法。考察了缓冲液种类、缓冲液p H、缓冲液浓度、分离电压、柱温、检测波长对分离的影响。在最佳条件40 mmol/L硼砂盐缓冲体系p H 9.35,分离电压25 k V,柱温20℃,检测波长为200 nm,七种防腐剂14 min内就完全达到分离。采用外标法定量,在0.6~240μg/m L内,回归方程相关系数0.9990~0.9998,检出限为0.07~0.14μg/m L,迁移时间和峰面积相对标准偏差(RSD)分别小于0.44%和2.0%,对实际样品测定,样品回收率为79.6%~120.3%。
A high performance capillary electrophoresis (HPCE) was developed for the simultaneous determination of benzoic acid, sorbic acid, dehydroacetic acid and methyl paraben, ethyl paraben, propyl paraben and butyl paraben in beverages method. The effects of buffer type, buffer pH, buffer concentration, separation voltage, column temperature, and detection wavelength on the separation were investigated. Under the optimum conditions, the buffer solution pH = 9.3, the separation voltage of 25 kV, the column temperature of 20 ℃ and the detection wavelength of 200 nm, the seven preservatives were completely separated within 14 min. The correlation coefficient of regression equation was 0.9990 ~ 0.9998 with the detection limit of 0.07 ~ 0.14μg / m L and the relative standard deviation (RSD) of migration time and peak area were less than 0.44% in the range of 0.6 ~ 240μg / And 2.0% respectively. The recovery of the sample was 79.6% ~ 120.3% for the actual samples.