格列齐特片(Ⅱ)含量测定和有关物质检测方法改进

Improvement in the Methods for Content and Related Substances Determination of Glielazide Tablets(Ⅱ)

关键词:  格列齐特片(Ⅱ)  含量测定  有关物质

Key words:  Glielazide tablets(Ⅱ)  content determination  related substance

摘要:

目的 解决中国药典2010年版收载的格列齐特片(Ⅱ)药品标准中含量测定和有关物质检测方法中供试溶液不稳定的问题。方法 以乙腈取代40%乙腈水溶液为溶剂配制供试品溶液，采用C₁₈色谱柱(250 mm×4.6 mm，5 μm)，流动相为水-乙腈-三乙胺-三氟醋酸(60∶40∶0.1∶0.1)，流速为1.5 mL·min^-1，柱温为35 ℃，检测波长为235 nm，样品盘温度为室温。结果 格列齐特片(Ⅱ)含量测定和有关物质检测项下各供试溶液在24 h内稳定。含量测定在20~500 mg·L^-1内线性关系良好，r值为0.999 9，加样回收率为100.1%，分析方法的定量下限为0.5 mg·L^-1，检测限为0.1 mg·L^-1。结论 该方法解决了原标准中供试溶液极不稳定的弊端，提高了检测结果的可信度和检测效率。

Abstract:

OBJECTIVE To improve the methods for content and related substances determination of Glielazide tablets(Ⅱ) METHODS The test solutions were made by acetonitrile instead of 40% acetonitrile aqueous solution. Chromatography was carried on a C₁₈ column(250 mm×4.6 mm, 5 μm) with the column temperature at 35 ℃, using water-acetonitrile-triethylamine- tirfluoroacetic acid(60∶40∶0.1∶0.1) as mobile phase at a flow rate of 1.5 mL·min^-1. The detective wavelength was set at 235 nm. The sample tray was at room temperature. RESULTS The test solutions of Glielazide tablets(Ⅱ) were stable in 24 h. The method had good linear relationships in 20-500 mg·L^-1(r=0.999 9), average recovery was 100.1%. The limits of quantitation and detection were 0.5 mg·L^-1 and 0.1 mg·L^-1, respectively. CONCLUSION The method improves the efficiency and reliability of test by resolving the problem of instability in the original standard.