Yin Changna, Cao Yuhua, Ding Shaodong, Wang Yun
School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, China.
J Chromatogr A. 2008 Jun 6;1193(1-2):172-7. doi: 10.1016/j.chroma.2008.04.016. Epub 2008 Apr 15.
A rapid, reliable and reproducible method based on microemulsion electrokinetic chromatography (MEEKC) for simultaneous determination of 13 kinds of water- and fat-soluble vitamins has been developed in this work. A novel microemulsion system consisting of 1.2% (w/w) sodium lauryl sulphate (SDS), 21% (v/v) 1-butanol, 18% (v/v) acetonitrile, 0.8% (w/w) n-hexane, 20mM borax buffer (pH 8.7) was applied to improve selectivity and efficiency, as well as shorten analysis time. The composition of microemulsion used as the MEEKC running buffer was investigated thoroughly to obtain stable separation medium, as well as the optimum determination conditions. Acetonitrile as the organic solvent modifier, pH of the running buffer and 1-butanol as the co-surfactant played the most important roles for the separation of the fat-soluble vitamins, water-soluble vitamins and stabilization of system, respectively. The 13 water- and fat-soluble vitamins were baseline separated within 30 min. The system was applied to determine water- and fat-soluble vitamins in commercial multivitamin pharmaceutical formulation, good accuracy and precision were obtained with recoveries between 97% and 105%, relative standard derivations (RSDs) less than 1.8% except vitamin C, and acceptable quantitative results corresponding to label claim.
本文建立了一种基于微乳液电动色谱（MEEKC）的快速、可靠且可重复的方法，用于同时测定13种水溶性和脂溶性维生素。开发了一种新型微乳液体系，其由1.2%（w/w）十二烷基硫酸钠（SDS）、21%（v/v）正丁醇、18%（v/v）乙腈、0.8%（w/w）正己烷、20mM硼砂缓冲液（pH 8.7）组成，该体系用于提高选择性和效率，并缩短分析时间。对用作MEEKC运行缓冲液的微乳液组成进行了深入研究，以获得稳定的分离介质以及最佳测定条件。乙腈作为有机溶剂改性剂、运行缓冲液的pH值以及正丁醇作为助表面活性剂，分别对脂溶性维生素的分离、水溶性维生素的分离以及体系的稳定性起着最重要的作用。13种水溶性和脂溶性维生素在30分钟内实现了基线分离。该体系应用于测定市售多种维生素药物制剂中的水溶性和脂溶性维生素，获得了良好的准确度和精密度，回收率在97%至105%之间，除维生素C外相对标准偏差（RSD）小于1.8%，且定量结果与标签标示量相符。
