高效液相色谱电化学检测法在硫酸阿奇霉素含量测定和有关物质概况分析上的应用

目的　建立硫酸阿奇霉素含量测定和有关物质概况分析的 HPL C电化学检测法。方法　采用 L ichro-CART1 2 5 - 4Aluspher RP- select B柱进行分离 ;HP1 0 4 9A型安培电化学检测器检测 ;最佳检测电势 +0 .6 V;流动相为磷酸二氢钾缓冲液 -乙腈 (2 1 30∶ 870 ) ,p H 1 1 .0± 0 .1 ;流速 1 .0 m L· min-1 ;柱温 5 0℃。结果　被测样品中明显检出多个杂质峰 ;硫酸阿奇霉素主峰的峰面积与进样量在 0 .0 2～ 1 .2 μg的范围内呈良好的线性关系 ,r =0 .9997。最低检测限为 1 ng;中间精密度试验日内差为 RSD 1 .1 % ;日间差为 RSD 0 .7%。结论　本法具有较高的灵敏度、精密度和专属性 ,适用于硫酸阿奇霉素含量测定以及有关物质的概况分析

Determination for potency and impurity profile of azithromycin sulfate by HPLC-ECD

Objective To establish an HPLC method to determine the potency of azithromycin sulfate and its impurity profile. Method The separation was performed on a LichroCART 125 4 Aluspher RP select B column (4 6×100 mm); The mobile phase was composed of monobasic potassium phosphate buffer solution acetonitrile (2130∶870), then the pH value was adjusted to 11 0±0 1; The detection was carried out on an HP1049A amperometric electrochemical detector with electrodes set at a optimized detection potential of +0 6 volt; The flow rate was 1 mL·min -1 and the column temperature was held on 50℃. Results Some impurities were obviously separated under the chromatographic system described above; the calibration curve of the peak responses vs. the amount injected was linear between 0 02～1 2 μg(r=0 999 7). The limit of detection was about 1ng; The RSD for repetition of the method within day was 1 1%, and the RSD among days was 0 7%. Conclusion This HPLC method offered a sensitive, rapid, repeatable and accurate procedure suitable for determining the potency of azithromycin sulfate and its impurity profile.