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目的:建立高效液相色谱法测定阿仑膦酸钠维生素D3片中维生素D3含量及有关物质。方法:用二甲基亚砜-水(10:2,含0.02%丁羟甲苯(BHT))为溶解介质,用含0.02%BHT的正己烷提取制剂中的维生素D3及其有关物质,采用Agilent ZORBAX RX-SIL色谱柱(Analytical 4.6mm×250mm,5μm),正己烷∶正戊醇(997∶3)为流动相,流速1.0mL.min-1,264nm为检测波长,柱温30℃。结果:维生素D3色谱峰与其相邻杂质峰能完全分离,维生素D3在3.5～10.5μg.mL-1范围内具有良好的线性关系(r=0.9997);回收率为98.72%,RSD为1.10%。精密度RSD为0.47%。结论:该法简便、灵敏、专属性强,适用于含微量维生素D3制剂的质量控制要求。
Objective: To establish a HPLC method for the determination of vitamin D3 in alendronate vitamin D3 tablets and related substances. METHODS: Vitamin D3 and its related substances were extracted with n-hexane containing 0.02% BHT with dimethylsulfoxide-water (10: 2, 0.02% butylated hydroxytoluene (BHT) ZORBAX RX-SIL column (Analytical 4.6 mm × 250 mm, 5 μm), n-hexane: n-amyl alcohol (997: 3) as mobile phase at a flow rate of 1.0 mL · min- Results: Vitamin D3 peak was completely separated from the adjacent impurity peak. Vitamin D3 showed a good linear relationship (r = 0.9997) in the range of 3.5 ~ 10.5μg.mL-1. The recovery rate was 98.72% and the RSD was 1.10%. The RSD of precision is 0.47%. Conclusion: The method is simple, sensitive and specific, suitable for the quality control requirements of trace vitamin D3 preparations.