Smidt C R, Jones A D, Clifford A J
Department of Nutrition, University of California, Davis 95616.
J Chromatogr. 1988 Dec 29;434(1):21-9. doi: 10.1016/0378-4347(88)80058-6.
An improved gas chromatographic method for the analysis of retinol and alpha-tocopherol in biological samples is described. The use of cold on-column injection in combination with wall coated open tubular column gas chromatography eliminates thermal decomposition of vitamin A and yields efficient separations of fat-soluble vitamins (A, D2, D3, and E) without derivatization. Peak tailing was judged to be minimal. Vitamins were quantified by flame ionization detection responses down to 3.5 ng injected, and their identities were confirmed using gas chromatography-mass spectrometry. Extracts of biological samples were saponified, and sterols were removed using digitonin-impregnated celite chromatography before analysis by gas chromatography and gas chromatography-mass spectrometry. Recoveries of vitamins from a test diet ranged from 89 to 103%.
本文描述了一种用于分析生物样品中视黄醇和α-生育酚的改进气相色谱法。采用冷柱头进样结合壁涂开管柱气相色谱法，可消除维生素A的热分解，并能在不进行衍生化的情况下有效分离脂溶性维生素（A、D2、D3和E）。峰拖尾现象被判定为最小。通过火焰离子化检测响应，对低至3.5 ng进样量的维生素进行定量，并使用气相色谱-质谱联用仪确认其身份。生物样品提取物经皂化处理，在进行气相色谱和气相色谱-质谱联用分析之前，使用洋地黄皂苷浸渍的硅藻土色谱法去除甾醇。从测试饮食中回收维生素的范围为89%至103%。
