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δ2.04处,多硫酸软骨素的乙酰甲基特征峰在δ2.15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).
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 δ 2.04 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.
出处
《波谱学杂志》
CAS
CSCD
北大核心
2011年第2期278-289,共12页
Chinese Journal of Magnetic Resonance
基金
国家火炬计划资助项目(2008GH021318)
