色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1275-1279.DOI: 10.3724/SP.J.1123.2014.07012

• 技术与应用 • 上一篇    下一篇

离子色谱法测定三磷酸腺苷二钠制剂中主成分及有关物质的含量

山广志1, 宗艳平1,3, 王晓2, 卢静华3   

  1. 1. 中国医学科学院医药生物技术研究所, 北京 100050;
    2. 烟台东诚药业集团股份有限公司, 山东 烟台 264006;
    3. 辽宁医学院药学院, 辽宁 锦州 121000
  • 收稿日期:2014-07-04 修回日期:2014-07-30 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 山广志,E-mail:Shanguangzhi@imb.pumc.edu.cn.
  • 基金资助:

    科技部新药创制重大专项平台项目(2012ZX09301002-001-019).

Determination of principal components and related substances in adenosine disodium triphosphate preparation by ion chromatography

SHAN Guangzhi1, ZONG Yanping1,3, WANG Xiao2, LU Jinghua3   

  1. 1. Institute of Medicinal Biotechnology, Chinese Academy of Medical Sciences, Beijing 100050, China;
    2. Yantai Dongcheng Pharmaceutical Group Co., Ltd., Yantai 264006, China;
    3. College of Medicine, Liaoning Medical University, Jinzhou 121000, China
  • Received:2014-07-04 Revised:2014-07-30 Online:2014-11-08 Published:2014-10-31

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摘要：

建立了用于三磷酸腺苷二钠制剂中主成分及有关物质含量测定的离子色谱方法。采用IonPac AS11-HC色谱柱,以KOH溶液为淋洗液,梯度洗脱,流速为1.0 mL/min,进样10 μL,以Dionex AERS 500 4-mm抑制器的电导检测器检测,三磷酸腺苷二钠(ATP-Na2)的含量按峰面积以外标法计算,二磷酸腺苷二钠(ADP-Na2)及单磷酸腺苷二钠(AMP-Na2)按加校正因子的主成分自身对照法计算,未知杂质按主成分自身对照法计算。ATP-Na2、ADP-Na2及AMP-Na2的线性范围分别为0.000146~1.83 g/L、0.000484~1.51 g/L及0.000426~0.804 g/L,相关系数分别为0.9997、0.9996及0.9999;对照品溶液在24 h内的稳定性良好(峰面积RSD分别为1.3%、1.4%、2.5%);ATP-Na2、ADP-Na2、AMP-Na2的方法定量限(S/N=10)分别为1.5 ng、4.8 ng、4.3 ng,检出限(S/N=3)分别为0.58 ng、1.21 ng、1.28 ng;ATP-Na2在3个水平的加样回收率分别为96.50%、96.57%和96.77%。本方法适用于三磷酸腺苷二钠制剂的质量控制。

关键词: 电导检测器, 离子色谱法, 三磷酸腺苷二钠, 有关物质, 制剂

Abstract:

A new method was developed for the determination of adenosine disodium triphosphate (ATP-Na2) and its related substances in ATP-Na2 preparation by ion chromatography (IC). The sample was diluted with ultrapure water and filtrated by 0.22 μm polyether sulfone filter membrance, and then analyzed by IC directly without any more pretreatment. The analysis was performed on a Dionex IonPac AS11-HC column(250 mm×4 mm) and a guard column IonPac AG11-HC (50 mm×4 mm). A KOH eluent generator cartridge was used for gradient elution at the flow rate of 1.0 mL/min. The detection was performed by a Dionex suppressed (Dionex AERS 500 4-mm) conductivity detector. The injection volume was 10 μL. The assay was quantitatively completed by external standard method and the related substances were calculated with correction factors. The linear ranges of the method for ATP-Na2, adenosine disodium diphosphate (ADP-Na2) and adenosine disodium monophosphate (AMP-Na2) were 0.000146-1.83 g/L (r=0.9997), 0.000484-1.51 g/L (r=0.9996) and 0.000426-0.804 g/L (r=0.9999), respectively. The average recoveries of ATP-Na2 were 96.50%, 96.57% and 96.77% at three spiked levels. The limits of quantitation (S/N=10) of ATP-Na2, ADP-Na2 and AMP-Na2 were 1.5 ng, 4.8 ng, 4.3 ng, and the limits of detection (S/N=3) were 0.58 ng, 1.21 ng, 1.28 ng, respectively. The results demonstrated that the system has the advantages of high sensitivity, facile automation and simple sample pretreatment. The method is suitable for the quality control of adenosine disodium triphosphate preparations.

Key words: adenosine disodium triphosphate (ATP-Na2), conductivity detector, ion chromatography (IC), preparation, related substances

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