维生素B1有关物质检测方法的研究与应用

Research and Application of Detection Methods for Vitamin B1 Related Substances

关键词:  维生素B₁  维生素B₁片  有关物质  高效液相色谱法

Key words:  vitamin B₁  vitamin B₁ tablets  related substances  HPLC

摘要:

目的 建立一种高效液相色谱法对维生素B₁片剂和原料药有关物质进行检测。方法 采用Waters液相色谱柱Symmetry C₁₈（250 mm×4.6 mm，5 μm），流动相A为4.045 g·L^-1庚烷磺酸钠溶液（含1%三乙胺，用磷酸调节pH至3.5），流动相B为甲醇-乙腈（1：1），采用梯度洗脱，波长为254 nm，流速为1.0 mL·min^-1。结果 分离度溶液中各杂质之间分离度均>1.5，片剂辅料不干扰8个已知杂质出峰，各已知杂质检测限为0.005~0.015 μg·mL^-1；在高温、高湿、光照条件下杂质H和未知杂质均有不同程度增长。结论 该方法可以同时运用于维生素B₁原料药和片剂的有关物质检测，维生素B₁片应在阴凉干燥避光的条件下保存。

Abstract:

OBJECTIVE To establish an HPLC method for the determination of vitamin B₁ tablets and active pharmaceutical ingredient related substances. METHODS Waters liquid chromatography column Symmetry C₁₈(250 mm×4.6 mm, 5 μm) was used. Mobile phase A was 4.045 g·L^-1 sodium heptane sulfonate solution (containing 1% triethylamine, pH adjusted to 3.5 with phosphoric acid), mobile phase B was methanol-acetonitrile (1:1). Gradient elution was used with a wavelength of 254 nm and a flow rate of 1.0 mL·min^-1. RESULTS The resolution of each impurity in the resolution solution was >1.5. Excipients in tablets didn't interfere with the peaks of 8 known impurities. Limit of detection of each impurity was in the range of 0.005-0.015 μg·mL^-1. It was found that the impurity H and the unknown impurity increased in different degrees under various conditions. CONCLUSION The method can be applied to the detection of related substances of vitamin B₁ active pharmaceutical ingredient and tablets. Vitamin B₁ tablets shall be stored under the conditions of cool, dry and dark.