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高效液相色谱法测定地西泮直肠凝胶有关物质

Determination of related substances in diazepam rectal gel by high-performance liquid chromatography

    摘要
  • 摘要:
    目的 建立一种高效液相色谱法, 用于测定地西泮直肠凝胶中的有关物质。
    方法 采用Agilent ZORBAX Eclipse Plus C18(4.6 mm×150.0 mm, 3.5 μm)色谱柱，以10 mmol/L磷酸二氢钾缓冲液(用0.5 mmol/L氢氧化钠溶液调节pH值至6.0)-甲醇为流动相，进行梯度洗脱，流速为1.0 mL/min, 柱温为30 ℃, 检测波长为234 nm。
    结果 地西泮与已知杂质Ⅰ~Ⅶ的色谱峰具有良好的分离度; 地西泮和已知杂质Ⅰ、Ⅱ、Ⅲ、Ⅳ分别在0.01~10.05 μg/mL和0.01~9.92 μg/mL、0.01~10.24 μg/mL、0.01~10.18 μg/mL、0.01~10.24 μg/mL范围内呈现良好的线性关系(r2≥0.999), 且其平均回收率均在99%~101%范围内。制剂中的辅料对主成分及有关物质的测定无干扰。
    结论 该高效液相色谱法专属性强，重复性好，适用于地西泮直肠凝胶中有关物质的检测。

     

    Abstract:
    Objective To establish a high-performance liquid chromatography method for the determination of related substances in diazepam rectal gel.
    Methods The Agilent ZORBAX Eclipse Plus C18 (4.6 mm×150.0 mm, 3.5 μm) column was used with a mobile phase consisting of 10 mmol/L potassium dihydrogen phosphate buffer (adjusted to pH value to 6.0 with 0.5 mmol/L sodium hydroxide solution) and methanol. Gradient elution was performed at a flow rate of 1.0 mL/min, with a column temperature of 30 ℃ and a detection wave length of 234 nm.
    Results The chromatographic peaks of diazepam and known impurities Ⅰ to Ⅶ showed good resolution. Diazepam and known impurities Ⅰ, Ⅱ, Ⅲ, and Ⅳ exhibited good linearity in the concentrations ranging of 0.01 to 10.05 μg/mL, 0.01 to 9.92 μg/mL, 0.01 to 10.24 μg/mL, and 0.01 to 10.18 μg/mL, respectively (r2≥0.999), with average recoveries ranging from 99% to 101%. The excipients in the formulation did not interfere with the determination of the principal component and related substances.
    Conclusion This high-performance liquid chromatography method is highly specific and reproducible, making it suitable for the detection of related substances in diazepam rectal gel.

     

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