HPLC测定醋酸奥曲肽及其制剂中的有关物质

Determination of related substances in Octreotide acetate and its preparation by HPLC

目的测定醋酸奥曲肽及其制剂的有关物质。方法采用YMC-Pack ODS-AQ C18色谱柱(250 mm×4.6 mm,5μm),流动相A为10%四甲基氢氧化铵溶液(取45 mL加水至800 mL,用磷酸溶液调pH2.0,再加水至900 mL)-乙腈(900:100),流动相B为10%四甲基氢氧化铵溶液(取45 mL加水至300 mL,用磷酸溶液调pH2.0,再加水至400 mL)-乙腈(400:600),流速1.5 mL·min^(-1),检测波长210 nm,柱温30℃,进样体积20μL。结果0.5022~10.0443μg·mL^(-1)奥曲肽与峰面积的线性关系良好,奥曲肽的检测限为2.5 ng,各杂质与奥曲肽峰均能完全分离。结论所用方法专属性好,可用于醋酸奥曲肽及其制剂的质量控制。

OBJECTIVE To determine the related substances of Octreotide acetate and its preparation.METHODS A YMC-Pack ODS-AQ C18(250 mm×4.6 mm,5μm)column was used.The mobile phase A was 10%tetramethylammonium hydroxide solution(45 mL in water to 800 mL,pH adjusted to 2.0 with phosphoric acid solution,add finally water added to 900 mL)-acetonitrile(900:100),and the mobile phase B was 10%tetramethylammonium hydroxide solution(45 mL,add water to 300 mL,pH adjusted to 2.0 with phosphoric solution,add finally water added to 400 mL)-acetonitrile(400:600).The flow rate was 1.5 mL·min^(-1).The detection wavelength was 210 nm.The column temperature was 30℃.Injection volume was 20μL.RESULTS The linear range of octreotide was 0.5022-10.0443μg·mL^(-1),and the detection limits of octreotide was 2.5 ng.The related substances and octreotide could be separated completely.CONCLUSION This method is specific and suitable for the quality control of octreotide acetate and its preparation.