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  

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

作　　者：林思荣 王勇 林晨 王磊 许永彬 石贞香 林芳 陈鼎雄 LIN Si-rong;WANG Yong;LIN Chen;WANG Lei;XU Yong-bin;SHI Zhen-xiang;LIN Fang;CHEN Ding-xiong(Fujian Institute for Food and Drug Quality Control,Fuzhou 350001,China;Jiangsu Taizhou Peopled Hospital,Taizhou 225300,China;Xiamen Institute for Food and Drug Quality Control,Xiamen 361012,China;Sinopharm Xingsha Pharm aceuticals(Xiamen)Co.,Ltd,Xiamen 361028,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350001 [2]江苏省泰州市人民医院,泰州225300 [3]厦门市食品药品质量检验研究院,厦门361012 [4]国药控股星鲨制药(厦门)有限公司,厦门361028

出　　处：《药物分析杂志》2021年第3期491-500,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：2018年度国家药品标准提高-维生素D含量测定法(二维色谱法)(2018Y006);福建省科学技术厅项目(2019Y0065)。

摘　　要：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D_(3)、维生素D_(3)的初步净化;以9 mL大体积的收集流路收集含有前维生素D_(3)、维生素D_(3)的组分,在第二维色谱完成前维生素D_(3)与维生素D_(3)的分离和定量。本方法可以直接分析2种制剂(维生素D滴剂和维生素AD滴剂),无需烦琐的样品制备程序。结果:2种制剂中维生素D_(3)在0.1008~0.9072μg·mL^(-1)浓度范围内线性关系良好,r=0.9997;重复性试验的RSD分别为0.4%、0.8%;平均回收率(RSD)分别为100.5%(0.78%)、100.7%(1.6%);检测下限为1.6 ng·mL^(-1),定量下限均为5.3 ng·mL^(-1);7批维生素D滴剂样品的维生素D_(3)含量范围在102.6%~111.8%,11批维生素AD滴剂样品的维生素D_(3)含量范围在97.4%~104.7%。结论:本实验建立的方法灵敏、准确,操作简单,对于油性和脂溶性维生素D制剂中维生素D_(3)的含量测定具有很好的应用前景。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 D_(3) and vitamin D_(3) were achieved in the first-dimensional liquid chromatography.The eluent containing pre-vitamin D_(3) and vitamin D_(3) 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 D_(3) and vitamin D_(3).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 D_(3) and vitamin D_(3) 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 D_(3) in 7 batches of vitamin D drops ranged from 102.6%to 111.8%.The contents of vitamin D_(3) 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 D_(3) in oily and fat soluble vitamin D preparations.

关 键 词：柱切换 二维液相色谱 前维生素D_(3) 维生素D_(3) 维生素D滴剂 维生素AD滴剂 含量测定 

分 类 号：R917[医药卫生—药物分析学]