hplc同时测定羟喜树碱注射液的有关物质及含量.pdfVIP

HPLC 同时测定羟喜树碱注射液的有关物质及含量 彭茗，陆丹，刘瑾，杨永健(上海市食品药品检验所，上海 201203) 摘要：目的 建立以高效液相色谱法同时测定羟喜树碱注射液的有关物质和含量的方法。方法 采用Ultimate XB-C 18 柱 1 (4.6 mm ×250 mm ，5 μm) ，流动相为甲醇-水(60 ∶40) ，检测波长为370 nm ，流速为1.0 mL·min ，柱温35 ℃。结果 有 关物质：羟喜树碱与杂质分离度良好，羟喜树碱和其主要杂质喜树碱的线性范围均在0.2~1.0 μg·mL1 之间，相关系数均 在0.999 7 以上，最低检测限分别为0.2 ng 和0.3 ng 。含量测定：羟喜树碱在4.0~36.3 μg·mL1 内线性相关系数为1.000 0， 根据3 个不同生产厂家的处方工艺分别进行低、中、高3 种浓度的回收率试验，结果均在 100.0%~102.0%之间，RSD 均 在0.02%~0.71%之间(n=3) 。结论 本方法专属性强、准确性高，可全面系统地控制羟喜树碱注射液的质量。 关键词：高效液相色谱法；羟喜树碱注射液；喜树碱；有关物质；含量测定 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2011)09-0866-05 Simultaneous Determination for Related Substances and Content of Hydroxycamptothecin Injection by HPLC PENG Ming, LU Dan, LIU Jin, YANG Yongjian(Shanghai Institute for Food and Drug Control, Shanghai 201203, China) ABSTRACT: OBJECTIVE To establish an HPLC method for simultaneous determination of related substances and content of hydroxycamptothecin injection. METHODS The chromatographic column was Ultimate XB-C 18(4.6 mm ×250 mm, 5 μm), and the mobile phase consisted of a mixture of methanol-water(60 ∶40). The flow rate was 1.0 mL·min1 and the detection wavelength was 370 nm. The column temperature was maintained at 35 ℃。RESULTS For the determination of related substances: the separations between hydroxycamptothecin and its related substances were very well. The calibration curves of hydroxycamptothecin and its main related substance, namely camptothecinthe, were both linear within the ranges of 0.21.0 μg·mL1(r ≥0.999 7), and the LODs were 0.2 ng and 0.3 ng, respectively. For the determination of content: hydroxycamptothecin was linear within