柱切换高效液相色谱法测定维生素D滴剂、维生素AD滴剂中维生素D的含量

目的:建立用于快速测定维生素D滴剂、维生素AD滴剂中维生素D含量的柱切换二维液相色谱方法.方法:样品用正己烷溶解后直接注入液相色谱系统,在第一维色谱完成前维生素D3、维生素D3的初步净化;以9 mL大体积的收集流路收集合有前维生素D3、维生素D3的组分,在第二维色谱完成前维生素D3与维生素D3的分离和定量.本方法可以直...

Determination of vitamin D content in vitamin D drops and vitamin A D drops by column-switching high-performance liquid chromatography

Objective:To develop a rapid method for direct determination of vitamin D in vitamin D drops and vitamin A D drops using two-dimensional column switch liquid chromatography.Methods:The sample was dissolved in n-hexane and injected directly into the liquid chromatography system.Preliminary purification of pre-vitamin D₃ and vitamin D₃ were achieved in the first-dimensional liquid chromatography.The eluent containing pre-vitamin D₃ and vitamin D₃ from the first dimensional column was collected by a 9 mL collection pipe and then switched into the second dimensional column to complete quantification of pre-vitamin D₃ and vitamin D₃.Two kinds of liquid vitamin D supplements(vitamin D drops and vitamin A and D drops)were directly analyzed using this system without any complicated preparation procedure.Results:The linear range of pre-vitamin D₃ and vitamin D₃ in vitamin D drops and vitamin A and D drops was 0.1008-0.9072μg·mL^-1 with the correlation coefficient of 0.9997.The RSDs of repeatability were 0.4% and 0.8%.The average recoveries were 100.5%(RSD=0.78%)and 100.7%(RSD=1.6%).The LOD was 1.6 ng·mL^-1 and LOQ was 5.3 ng·mL^-1.The contents of vitamin D₃ in 7 batches of vitamin D drops ranged from 102.6%to 111.8%.The contents of vitamin D₃ in 11 batches of vitamin A D drops ranged from 97.4%to 104.7%.Conclusion:The method is sensitive,accurate and easy to operate.It has a good application prospect for the determination of vitamin D₃ in oily and fat soluble vitamin D preparations.