高效毛细管电泳法同时分离检测肝素钠杂质

 目的 建立用高效毛细管电泳法同时分离检测肝素钠杂质的方法。方法 采用高效毛细管电泳法，通过选择电极缓冲液的种类、浓度、pH值、检测波长等最佳实验条件，确定了一种检测肝素钠杂质的优化方法：800 mmol·L-1磷酸-锂盐为运行缓冲液(pH 3.5)，熔融石英毛细管(25 μm×60 cm，有效长度50 cm)，分离电压-30 kV，进样量：14 kPa×50 s，分离温度：20 ℃，检测波长200 nm。结果 此方法实现了肝素钠与各个杂质的分离，多硫酸软骨素(oversulfated chondroitin sulfate, OSCS)峰和肝素峰的分离度可达1.5，且线性、重复性良好，OSCS峰检测限为0.2 mg·mL-1，相当于肝素钠质量的0.4%（Woscs/Wheparin）。结论 此方法准确、简便，优于美国药典(USP 32)收载的方法，利于肝素钠的质量控制。

Separation and Determination of Impurities in Heparin Sodium Simultaneously by Capillary Electrophoresis

OBJECTIVE To screen the optimal formulation and preparation of trihydroxybenzoic acid (TBA) liposomes， and establish a HPLC method for the determination of the content and entrapment efficiency of TBA liposomes. METHODS TBA liposomes were prepared by the ultrasonic membrance method. The content of TBA and the entrapment efficiency were detected by HPLC. The analytical column was an Agilent TC-C₁₈ column（4.6 mm×150 mm，5 μm）.The mobile phase was methanol-0.1% phosphoric acid（15∶85）.The flow rate was 0.8 mL·min-1.The detection wavelength was 273 nm. RESULTS TBA showed good linerity over the range fo 50-150 mg·L-1 (r=0.998 0，n=5）.The average recovery was 98.25%(RSD=0.45%).CONCLUSION The entrapment efficiency of TBA liposomes which was prepared by this method is up to the requirement. HPLC was proved to be simple， accurate， sensitive and applicable.