目的 对生长抑素及制剂有关物质测定方法进行了优化,并建立了生长抑素及制剂的含量测定方法。方法 通过与2020年版《中国药典》标准方法对比,流速、检测波长等参数的选择,色谱柱的筛选,对生长抑素及制剂的有关物质方法进行了优化;建立了生长抑素及制剂的含量测定方法,并进行了方法学验证。结果 优化后的有关物质测定方法能够将主成分与相邻杂质有效的分离;建立的含量测定方法,生长抑素的检测限为0.01 μg,定量限为0.02 μg,线性范围为0.01~0.5 mg·mL^-1(r=0.999 9),平均回收率(n =3)为100.2%(RSD=0.996%)。结论 优化后的有关物质测定方法更为灵敏、测定结果更准确;建立的含量测定方法高效、快速、灵敏、准确,可对生长抑素及制剂的含量进行质控,本研究为《中国药典》标准的修订提供方法依据。

OBJECTIVE To optimize determination method of related substances in somatostatin and preparation, and to establish content determination method of somatostatin and preparation. METHODS Through the comparison of pharmacopoeia standard methods, the selection of flow rate, detection wavelength and other parameters, the selection of chromatographic column, the determination method of related substances in somatostatin and preparation were optimized. A method for the content determination of somatostatin and its preparation was established and validated. RESULTS The optimized method can effectively separate the main components from the adjacent impurities. The limits of detection and quantitation were 0.01 μg and 0.02 μg, respectively. The linear range was 0.01 mg· mL^-1 to 0.5 mg· mL^-1(r=0.999 9). The average recovery(n=3) was 100.2%(RSD=0.996%). CONCLUSION The optimized method is more sensitive and accurate. The established content determination method is efficient, rapid, sensitive and accurate, and can be used for quality control of somatostatin and preparation. This study provides a basis for revising pharmacopoeia standards.