甘露聚糖肽HPLC法指纹图谱的建立

Establishment of Fingerprint in Mannatide by HPLC

采用HPLC法建立甘露聚糖肽口服液中氨基酸指纹图谱。色谱条件为Diamonsil C18柱(250mm×4.6mm,5μm),流动相:A相为乙腈-水(4∶1),B相为0.1mol/L醋酸钠-乙腈(93∶7,pH6.4);梯度洗脱;流速1.0mL/min;检测波长254nm。以异硫氰酸苯酯为衍生化试剂,对来自3个厂家共10批次产品进行色谱分析,建立甘露聚糖肽口服液指纹图谱。精密度、重现性、稳定性试验RSD均不大于3%。未水解甘露聚糖肽口服液指纹图谱共有11个峰,水解后指纹图谱共有11个峰,样品相似度均在0.90以上。研究结果表明,本方法稳定、准确,可为控制甘露聚糖肽口服液的质量提供参考。

Determination of fingerprint and technical parameter of amino acids in mannatide oral solution were conducted with high performance liquid chromatography method.Chromatographic conditions：Separa-tions were performed on a Diamonsil C18 column （250 mm×4.6 mm,5μm）,Mobile phase A：acetonitrile-water（4∶1）,mobile phase B：0.1 mol/L acetate-acetonitrile（93∶7,pH6.4）;gradient elution;flow rate：1.0 mL/min;detection wavelength：254 nm.With phenylisothiocyanate as derivative agent,ten samples from different mannatide oral solution of three factory were analyzed and evaluated,the fingerprint of ami-no acids in mannatide oral solutions were determinated.The relative standard deviation （RSD）of precision and reproducibility was not more than 3%.There were 1 1 cornmorl peaks in non-hydrolyzed sample of fin-gerprint,1 1 conllnon peaks in hydrolyzed sample of fingerprint.The similarity of samples was all above 0.90.The result showed that the method is accurate,convenient,stable,and the chromatographic finger-prints can be served as a powerful tool for the further quality control of mannatide oral solution.