Kobayashi T, Adachi A
J Nutr Sci Vitaminol (Tokyo). 1976;22(1):41-51. doi: 10.3177/jnsv.22.41.
Gas-liquid chromatographic (GLC) determination of vitamin D in multivitamin preparations was investigated and a simple routine method was established. The unsaponifiable matters of a sample was applied to a thin-layer chromatography (TLC) plate using Kieselgel GF254 as an adsorbent and a mixture of n-hexane-ethyl acetate (4:1) as a developing solvent. The scraped zones corresponding to vitamin D and previtamin D were extracted and determined by GLC using 1.5% OV-17 packed on Shimalite W (80-100 mesh) as a stationary phase. When the proposed method was applied to model preparations made by mixing vitamin D, A and E, it was confirmed that the determination of vitamin D was possible when the ratios of vitamin A and E (DL-alpha-tocopheryl acetate) to vitamin D were within 104 (I.U. ratio) and 2,500 (weight ratio), respectively. Since the ratios of most of commercial multivitamin preparations on sale in Japan are within the limitations and the results on multivitamin preparations were also satisfactory, the proposed method was confirmed to be suitable simple routine.
研究了气相色谱法（GLC）测定多种维生素制剂中维生素D的方法，并建立了一种简单的常规方法。将样品的不皂化物点样于以硅胶GF254为吸附剂、正己烷 - 乙酸乙酯（4:1）混合液为展开剂的薄层色谱（TLC）板上。刮下对应于维生素D和前维生素D的区域，以涂覆于Shimalite W（80 - 100目）上的1.5% OV - 17为固定相，用GLC进行测定。当将该方法应用于由维生素D、A和E混合制成的模拟制剂时，证实当维生素A和E（DL-α-生育酚乙酸酯）与维生素D的比例分别在104（国际单位比）和2500（重量比）以内时，维生素D的测定是可行的。由于日本市场上销售的大多数市售多种维生素制剂的比例都在该范围内，且对多种维生素制剂的测定结果也令人满意，因此该方法被确认为是一种适用的简单常规方法。
