Takeuchi A, Okano T, Teraoka S, Murakami Y, Kobayashi T
J Nutr Sci Vitaminol (Tokyo). 1984 Feb;30(1):11-25. doi: 10.3177/jnsv.30.11.
A simplified and accurate method for the determination of vitamin D in foods, feeds and pharmaceuticals was established by high-performance liquid chromatography (HPLC) using successively reversed-phase and straight-phase columns. About 1-2 g of a sample was accurately weighed and directly saponified. The extracted unsaponifiable matter was subjected to preparative HPLC using a reversed-phase column and a vitamin D fraction was collected. The fraction was subsequently subjected to analytical HPLC using a straight-phase column and vitamin D was assayed by estimating the peak height. The proposed method was applied to various kinds of samples, e.g., fishery products, fish meals, mixed feeds for fish farming and chicken farming, egg yolk, milk products, cattle liver, Shiitake, fortified foods and multivitamin preparations. The results showed that the proposed method was useful for the determination of vitamin D in such samples, because the peak of vitamin D in the profile of the second HPLC was always clearly separated from other concomitants and good recovery was obtained. Therefore, we think that the method is useful as a routine one for the determination of vitamin D in foods, feeds and pharmaceuticals.
建立了一种使用反相柱和正相柱依次进行高效液相色谱(HPLC)测定食品、饲料和药品中维生素D的简化且准确的方法。准确称取约1 - 2 g样品并直接皂化。将提取的不皂化物用反相柱进行制备型HPLC,收集维生素D馏分。随后,该馏分用正相柱进行分析型HPLC,并通过估算峰高测定维生素D。该方法应用于各种样品,如渔业产品、鱼粉、养鱼和养鸡的混合饲料、蛋黄、乳制品、牛肝、香菇、强化食品和多种维生素制剂。结果表明,该方法对于测定此类样品中的维生素D很有用,因为第二次HPLC图谱中维生素D的峰总是能与其他共存物清晰分离,并且回收率良好。因此,我们认为该方法作为测定食品、饲料和药品中维生素D的常规方法很有用。