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

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,5μm),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0.005~0.015μg×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。

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,5μm)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 0.005-0.015μg×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.