波谱学杂志 ›› 2011, Vol. 28 ›› Issue (2): 278-289.

• 研究论文 • 上一篇    下一篇

1H NMR分析肝素钠中杂质多硫酸软骨素

高照明,张玉冰*   

  1. 生态化工教育部重点实验室,青岛科技大学 化学院,山东 青岛  266042
  • 收稿日期:2010-07-16 修回日期:2010-09-06 出版日期:2011-06-05 发布日期:2011-06-05
  • 基金资助:

    国家火炬计划资助项目(2008GH021318).

Assessment of Oversulfated Chondroitin Sulfate in Heparin Sodium Solution with 1H NMR

 GAO Zhao-Ming, ZHANG Yu-Bing*   

  1. Key Laboratory of Eco-chemical Engineering, Ministry of Education, College of CCME, Qingdao University of Science and Technology, Qingdao 266042, China
  • Received:2010-07-16 Revised:2010-09-06 Online:2011-06-05 Published:2011-06-05
  • Supported by:

    国家火炬计划资助项目(2008GH021318).

摘要:

对肝素钠、多硫酸软骨素标准品进行了1H NMR测试并对谱图进行了全归属,指出: 肝素钠乙酰甲基特征峰在δ 2.04处,多硫酸软骨素的乙酰甲基特征峰在δ 2.15处. 同时考察了精细测试的实验条件,结果表明:当样品浓度为25 mg/0.6 mL、定标物TSP含量为0.020%(W/V)、样品旋转为12 Hz、处理参数(LB)为1.0、仪器频率为500 MHz时,能快速并准确的检测出肝素钠中的污染物(多硫酸软骨素).  

关键词: 核磁共振(NMR), 定量分析, 肝素钠, 多硫酸软骨素

Abstract:

The standard samples of heparin (HP) and oversulfated chondroitin sulfate (OSCS) were analyzed by 1H NMR. The spectra were assigned. The results showed that the acetyl-methyl peaks of heparin and OSCS have different chemical shift, at δ2.04 and δ 2.15 respectively. The experimental conditions for quantitative analysis were studied. It was shown that, OSCS content in HP solution can be accurately measured under the following conditions: 25 mg sample in 0.6 mL D2O, 0.020%(W/V)TSP, spinning rate 12 Hz, line broadening for EM window functions 1.0, and spectrometer frequency of 500 MHz.

Key words: NMR, quantitative analysis, heparin sodium, OSCS 

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