HPLC检测维生素B2片中有关物质的方法优化

Improvement of Content Determination for Related Substances in Vitamin B2 Tablets by HPLC

关键词:  维生素B₂片  高效液相色谱法  有关物质  优化参数

Key words:  vitamin B₂ tablets  HPLC  related substances  optimize parameters

摘要:

目的 优化维生素B₂片中有关物质的检测方法。方法 采用Welch Ultimate AQ-C₁₈柱（4.6 mm×250 mm，5 μm），流动相为0.1%磷酸水溶液（A）-乙腈（B），进行梯度洗脱；流速为1.0 mL·min^-1；检测波长267 nm；柱温30℃。结果 各杂质与主成分峰分离度良好；杂质A在0.008 7~0.053 5 μg·mL^-1（r²=0.998 1）、杂质B在0.019 8~0.812 3 μg·mL^-1（r²=0.999 8）、杂质D在0.007 3~0.838 7 μg·mL^-1（r²=1.000 0）、维生素B₂在0.011 3~0.427 6 μg·mL^-1（r²=0.999 4）内呈现良好的线性关系；杂质A、杂质B、杂质D平均回收率（n=9）分别为100.1%（RSD=1.6%）、100.6%（RSD=2.0%）和101.1%（RSD=1.1%）。结论 本检测方法专属性强、准确度高，可用于控制维生素B₂片中的有关物质。

Abstract:

OBJECTIVE To optimize a method for related substances determination of vitamin B₂ tablets. METHODS The Welch Ultimate AQ-C₁₈ column(4.6 mm×250 mm, 5 μm) was used. The mobile phase A was 0.1% phosphoric acid solution and the mobile phase B was acetonitrile for gradient elution. The flow rate was 1.0 mL·min^-1. The detection wavelength was 267 nm. The column temperature was 30 ℃. RESULTS The separation of impurity and principal component peak was good. The calibration curves were linear, the impurity A in range 0.008 7-0.053 5 μg·mL^-1(r²=0.998 1), the impurity B in range 0.019 8-0.812 3 μg·mL^-1(r²=0.999 8), the purity D in range 0.007 3-0.838 7 μg·mL^-1 (r²=1.000 0) and vitamin B₂ 0.011 3- 0.427 6 μg·mL^-1(r²=0.999 4). The average recoveries of impurity A, impurity B and impurity D were 100.1%(RSD=1.6%), 100.6%(RSD=2.0%) and 101.1%(RSD=1.1%). CONCLUSION This detection method has strong specificity and high accuracy, and can be used to control related substances in vitamin B₂ tablets.