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1H NMR分析肝素钠中杂质多硫酸软骨素
引用本文:高照明,张玉冰.1H NMR分析肝素钠中杂质多硫酸软骨素[J].波谱学杂志,2011,28(2):278-289.
作者姓名:高照明  张玉冰
作者单位: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
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  
收稿时间:2010-07-16

Assessment of Oversulfated Chondroitin Sulfate in Heparin Sodium Solution with 1H NMR
GAO Zhao-ming,ZHANG Yu-bing.Assessment of Oversulfated Chondroitin Sulfate in Heparin Sodium Solution with 1H NMR[J].Chinese Journal of Magnetic Resonance,2011,28(2):278-289.
Authors:GAO Zhao-ming  ZHANG Yu-bing
Institution:Key Laboratory of Eco-chemical Engineering, Ministry of Education, College of CCME, Qingdao University of Science and Technology, Qingdao 266042, China
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.
Keywords:NMR  quantitative analysis  heparin sodium  OSCS  
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