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目的:针对缩宫素注射液现行标准中未对注射液中有关物质进行控制的情况,建立了缩宫素注射液有关物质的HPLC测定法,并对2010年国家评价性抽验中178批缩宫素注射液样品进行了测定。方法:采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm);以0.1 mol.L-1磷酸盐缓冲液作为流动相A,以水-乙腈(1∶1)作为流动相B,梯度洗脱,柱温40℃,流速为1.0 mL.min-1,检测波长为220 nm。结果:在本文色谱条件下,主峰和杂质峰能得到良好的分离;缩宫素在浓度0.36～23.04 IU.mL-1范围内峰面积与浓度呈良好线性关系,r=0.9999;平均回收率99.1%(n=9)。178批缩宫素注射液总杂质为25.9%～36.0%,单个最大杂质为6.1%～13.0%。结论:该法专属性强,灵敏、准确,可作为缩宫素注射液的质量控制方法。现行标准不能有效控制药品质量,体现在有关物质偏高。研究表明制剂中的有关物质部分是由原料引入,因此,必须修订并提高原料和制剂的质量标准,增加有关物质检查。建议原料生产企业采用固相合成工艺的缩宫素提高原料质量,加强生产过程中各个环节的质量意识。
OBJECTIVE: To establish a HPLC method for the determination of related substances in oxytocin injection for the purpose of not controlling the related substances in the injection in the current standard of oxytocin injection, Su-injection samples were measured. Methods: Agilent ZORBAX SB-C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase A was consisted of 0.1 mol·L-1 phosphate buffer and water-acetonitrile (1: Gradient elution, the column temperature 40 ℃, the flow rate of 1.0 mL.min-1, detection wavelength of 220 nm. Results: Under the chromatographic conditions, the main peak and impurity peak were well separated. The peak area of oxytocin showed a good linear relationship with the concentration in the range of 0.36 ~ 23.04 IU · mL-1, r = 0.9999. The average recovery was 99.1 % (n = 9). 178 oxytocin injection total impurities of 25.9% to 36.0%, the largest single impurity of 6.1% to 13.0%. Conclusion: The method is highly specific, sensitive and accurate and can be used as a quality control method for oxytocin injection. Current standards can not effectively control the quality of medicines, reflected in the high substance. Research shows that the relevant substances in the preparation are partly introduced from the raw materials. Therefore, the quality standards of the raw materials and preparations must be revised and increased to increase the related substances inspection. Proposed raw material production enterprises using solid-phase synthesis of oxytocin to improve the quality of raw materials, and strengthen the production process in all aspects of quality awareness.