在线二维柱切换-高效液相色谱法同时测定婴幼儿强化奶粉中维生素A、D_3和E的含量  

Simultaneous Qualification of Vitamins A,D_3 and E in Fortified Infant Formulae by Liquid Chromatography Coupled with Fully Automated Online Two-dimensional Column Switching Method

作　　者：张艳海 朱晓艳[2] 曹国洲[2] 杨新磊 张丽娟 金燕 

机构地区：[1]赛默飞世尔科技(中国)有限公司,上海201203 [2]宁波出入境检验检疫局,宁波315012

出　　处：《分析化学》2013年第5期771-775,共5页Chinese Journal of Analytical Chemistry

摘　　要：使用双梯度液相色谱系统紫外检测器,建立了二维液相色谱法全自动、快速、同时测定婴幼儿奶粉中维生素A,D3,E的含量。采用了非水反相系统,以Acclaim C18柱为一维分析柱,Acclaim PAⅡC18柱为二维分析柱。利用一维色谱柱完成维生素A和E的分离测定和维生素D的净化分离;利用二维色谱柱完成维生素D的分析。一维分析以乙腈-甲醇体系作为流动相,流速0.6 mL/min;二维分析以乙腈-异丙醇体系作为流动相,流速0.8 mL/min,梯度洗脱。检测波长为325,296和263 nm,采用波长切换方式,整个分析过程仅需28 min。维生素D3在20～2000μg/L范围内的相关系数r为0.9998,平均回收率为100.7%;维生素A在1.71～855 mg/L浓度范围内的相关系数r为0.9979,平均回收率为114%;维生素E在4.12～1030 mg/L范围内的相关系数r为0.9995,平均回收率为94.0%。本方法可快速准确测定婴幼儿乳品中维生素A、D3和E的含量。A novel automated method for simultaneous quantification of vitamins A, D3 and E in fortified infant formulae has been developed using two-dimensional column-switching chromatography with dual gradient liquid chromatography system coupled with UV detector. Non-aqueous reversed-phase chromatography was used in the method. The determination of vitamins A, E and the purification of vitamin D were accomplished in the one-dimensional column. The separation of vitamin D was finished on the two-dimensional column. Acclaim C^8 was used as one-dimensional column with mobile phase consisting of acetonitrile and methanol at the flow rate of 0.6 mL/min and Acclaim PAII C18 which was a little different from C18 was employed as two- dimensional column and the mobile phase was composed of acetonitrile and isopropyl alcohol at the flow rate of 0.8 mL/min. The detection wavelengths were set at 325, 296 and 263 nm for respective vitamin by using wavelength time-switching program. It takes 28 min to finish the total analytical progress. The good linearity of vitamins A, D3 and E was proved respectively in the range of 1.7-855 mg/L（r=0.9979）, 20-2000μg/L （r=0.9998） and 4. 12-1030 mg/L （r=0. 9995）. The mean recoveries of vitamins A, D3 and E were 114.0%, 100.9%, and 94.0% respectively. It was proved that this method could greatly improve the efficiency of sample analysis.

关 键 词：高效液相色谱 二维色谱柱 双样充系统 婴幼儿配方奶粉 维生素D 维生素A 维生素E 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.72[轻工技术与工程—食品科学与工程]