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 x 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。
Determination of related substances in diazepam rectal gel by high-performance liquid chromatography
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 x 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 so-dium 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 chromato-graphic 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,respec-tively(r2 ≥0.999),with average recoveries ranging from 99％to 101％.The excipients in the for-mulation did not interfere with the determination of the principal component and related substances.Conclusion This high-performance liquid chromatography method is highly specific and reproduci-ble,making it suitable for the detection of related substances in diazepam rectal gel.
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