色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱法测定头孢他啶的含量及杂质

姜恩铸1,2,胡昌勤1

  

  1. 1.National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050, China;
    2.Institute of Medicinal Biotechnology, Chinese Academy of Medical and
    Peking Union Medical College, Beijing 100050, China
  • 收稿日期:2007-07-04 修回日期:2007-09-18 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 胡昌勤

Determination of ceftazidime and impurities using high performance liquid chromatography

JIANG Enzhu1,2, HU Changqin1   

  1. 1.National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050, China;
    2.Institute of Medicinal Biotechnology, Chinese Academy of Medical and
    Peking Union Medical College, Beijing 100050, China
  • Received:2007-07-04 Revised:2007-09-18 Online:2008-01-30 Published:1984-09-25

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摘要：

采用高效液相色谱法测定了头孢他啶的含量及杂质。以Alltima C18色谱柱(250 mm×4.6 mm,5 μm)为分离柱,以乙腈和磷酸盐缓冲溶液(pH 3.9)分别为流动相A和流动相B进行梯度洗脱,流速1.3 mL/min,柱温35 ℃,紫外检测波长255 nm。从头孢他啶药物中共分出14个杂质,且14个杂质间具有良好的分离度。头孢他啶在0.267~1069 μg/mL范围内与峰面积具有良好的线性关系(r=1.0000);其定量限(S/N=10)和最低检出限(S/N=3)分别为3.1 ng和0.93 ng。3个浓度的日内测定值的相对标准偏差(RSD）为0.72%(n=3),日间测定值的RSD为0.91%(n=3)。头孢他啶溶液在4 ℃避光条件下放置24 h保持稳定。本方法与欧洲/英国药典和日本药局方的方法比较，具有分离杂质数量多、分离度好的优点。

关键词: 高效液相色谱法, 梯度洗脱, 头孢他啶, 杂质

Abstract:

A high performance liquid chromatographic （HPLC） method for the determination of ceftazidime and impurities in ceftazidime drug was developed and verified. An Alltima C18 column (250 mm×4.6 mm, 5 μm) was used as the analysis column. Acetonitrile and phosphate buffer (22.6 g/L aqueous solution of ammonium dihydrogen phosphate, adjusted to pH 3.9 with 10%(v/v) phosphoric acid) were used as mobile phases with gradient elution at a flow rate of 1.3 mL/min. The column temperature was kept at 35 ℃, and the detection wavelength was set at 255 nm. Fourteen impurities could be well separated. The assay exhibited a good linearity in the ceftazidime concentration range of 0.267-1069 μg/mL with a correlation coefficient of 1.0000. The limits of the quantitation and qualification of ceftazidime were 3.1 ng and 0.93 ng, respectively. The relative standard deviations (RSDs) of the interday and intraday （n=3） determinations at three concentration levels were 0.72% and 0.91%, respectively. At 4 ℃ ang under darkness, ceftazidime solution was stable for 24 h. The developed method is superior to the counterparts in British and Japanese pharmacopeias in the number of the impurities separated and detected.

Key words: ceftazidime, gradient elution, impurities , high performance liquid chromatography (HPLC)