HPLC测定愈创木酚磺酸钾的有关物质

Determination of the Related Substances of Potassium Guaiacolsulfonate by HPLC

关键词:  愈创木酚磺酸钾  有关物质  高效液相色谱法  异构体

Key words:  potassium guaiacolsulfonate  related substance  HPLC  isomer

摘要:

目的 建立HPLC测定愈创木酚磺酸钾有关物质的方法。方法 采用InertSustain C₁₈色谱柱（4.6 mm×250 mm，5 μm），以乙腈-0.02 mol·L^-1磷酸盐缓冲液（20∶80）为流动相，流速1 mL·min^-1，柱温35℃，检测波长279 nm。结果 愈创木酚磺酸钾的2个异构体能得到有效分离，主成分与杂质的分离度良好。主成分及其各杂质在各自浓度范围内呈现良好的线性关系（r>0.999）；异构体Ⅲ、愈创木酚和杂质Ⅰ的平均加样回收率分别为101.35%，100.78%，99.45%，RSD分别为0.7%，0.7%，1.4%。结论 该方法快速、准确、专属性强，可用于愈创木酚磺酸钾原料药的有关物质检查。

Abstract:

OBJECTIVE To establish an HPLC method for determination of the related substances of potassium guaiacolsulfonate. METHODS The analysis was performed on an InertSustain C₁₈ column(4.6 mmx250 mm, 5 mm) with the mobile phase consisted of acetonitrile-0.02 mol·L^-1 phosphate buffer(20:80). The flow rate was 1 mL·min^-1. The column temperature kept at 35℃, and the detection wavelength was 279 nm. RESULTS The separation between the two isomers of potassium guaiacolsulfonate could be effectively separated, and the separation between the main component and impurities was good. The calibration curves of potassium guaiacolsulfonate and known impurities were linear in the self-concentration range (r>0.999); and the average recoveries of isomerⅢ, guaiacol and impurity Ⅰwere 101.35%, 100.78%, 99.45%, while RSDs were 0.7%, 0.7%, 1.4%, respectively. CONCLUSION The method is rapid, accurate, sensitive and reliable for determination of the related substances of potassium guaiacolsulfonate.