摘要
目的根据硫酸氢氯吡格雷的波谱特征揭示其手性特征和多晶型差异。方法采用红外光谱、核磁共振、粉末X-衍射、比旋度和熔点测定等技术,检测了硫酸氢氯吡格雷的波谱特征、晶面间距,旋光度和熔点等。结果硫酸氢氯吡格雷的手性构型在NOESY谱中得到表达,且S型(+55.05°)的比旋度不同于R型(-55.40°);Ⅰ型晶和Ⅱ型晶在红外光谱波数568、590 cm-1表现出明显的差异,在粉末X-衍射的晶面间距出现多处差异,且Ⅰ型晶的熔点比Ⅱ型晶高8℃。结论具有典型手性结构和多晶结构的硫酸氢氯吡格雷通过多维核磁共振谱和比旋度测定表现出手性结构特征;通过红外光谱、粉末X-衍射和熔点可区分出晶型特征。
OBJECTIVE To reveal the chirality and polymorphs of Clopidogrel hydrogen sulfate according to its spectrum feature.METHODS On the basis of IR,NMR,XRD,specific optical rotation and melting point analyses,the sample’s spectrum,interplanar spacing,optical rotation and melting point were detected.RESULTS The stereo configuration of the sample was reflected in NOESY.Specific optical rotation of the sample,configuration S,was + 55.05°,differed from-55.4° of configuration R.Besides,the sample formⅠand formⅡ showed apparent difference in IR at the wave number of 568 cm-1 and 590 cm-1,and in several XRD interplanar spacing.Melting point of formⅠ was 8 ℃ higher than that of formⅡ.CONCLUSION Clopidogrel hydrogen sulfate is a typical example of both polymorphs and chiral structure.Chirality of Clopidogrel hydrogen sulfate can be explained through NOESY and specific optical rotation,and crystal form can be distinguished by IR,XRD and melting point.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2012年第4期359-361,共3页
West China Journal of Pharmaceutical Sciences
关键词
硫酸氢氯吡格雷
手性
多晶型
Clopidogrel hydrogen sulfate
Chirality
Polymorphs