反向高效液相色谱法快速测定维生素D类膳食补充剂中维生素D3含量

Rapid determination of vitamin D3 content in vitamin D dietary supplements by reversed phase high performance liquid chromatography

中文关键词:  反向高效液相色谱法  维生素D  二甲基亚砜  膳食补充剂  

英文关键词:reversed phase high performance liquid chromatography  vitamin D  dimethyl sulfoxide  dietary supplements

中文摘要:

      目的 建立反向高效液相色谱法(reversed phase high performance liquid chromatography, RP-HPLC), 快速测定维生素D类膳食补充剂中维生素D3 (vitamin D3, VD3)含量的方法。方法 试样经二甲基亚砜超声提取, 甲醇定容过膜后, 采用C18反相高效液相色谱柱分离, 以甲醇:水(95:5, V:V)为流动相, 紫外检测器检测, 外标法定量。结果 本方法的专属性良好, VD3质量浓度线性范围为0.0510~1.0195 μg/mL, 相关系数为0.9999; 检出限为0.002 μg/mL; 仪器精密度的相对标准偏差(relative standard deviation, RSD)为1.85%; 方法重复性的RSD为0.57%; 平均加标回收率为95.63%, RSD为4.53%; 供试品溶液在24 h稳定, RSD为0.57%; 方法耐用性测试良好。本方法与国家标准方法检测结果基本一致, 相对偏差范围为3.0%~3.8%。结论 本方法操作简便, 结果准确, 检测设备要求低, 适用于维生素D类膳食补充剂中VD3含量的快速测定, 可为相关产品的质量控制提供更优的技术支持。

英文摘要:

      Objective To establish a method for rapid determination of vitamin D3 (VD3) content in vitamin D dietary supplements by reversed phase high performance liquid chromatography (RP-HPLC). Methods The sample was extracted with dimethyl sulfoxide by ultrasonic wave, and then passed through a membrane with methanol to make up the volume. It was separated by a C18 chromatographic column with methanol:water (95:5, V:V) as the mobile phase, detected by ultraviolet detector, and quantified by external standard method. Results The specificity of this method was good. The linear range of VD3 mass concentrations was 0.0510–1.0195 μg/mL, and the correlation coefficient was 0.9999. The limit of detection was 0.002 μg/mL. The relative standard deviation (RSD) of the instrument precision was 1.85%. The RSD of the method precision was 0.57%. The average recovery rate was 95.63%, and the RSD was 4.53%. The solution of test sample was stable in 24 hours, and the RSD was 0.57%. The durability of this method was good. The test result of this method was basically consistent with the test result of the national standard method, with a relative deviation range of 3.0%–3.8%. Conclusion The established method is simple, accurate and low requirements for testing equipment, which is suitable for rapid determination of the VD3 in vitamin D dietary supplements. The method can provide better technical support for the quality control of related products.