主题:固体核磁共振的CP/MAS实验能进行定量分析吗?

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ausky
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请教各位老师,谢谢!
推荐答案:celan回复于2005/09/03

Solid-state carbon NMR 可以定量,请看下面的文章.该文研究的是一种药物roxifiban,我把它的结构也帖出来供参考.
Title
Solid-state carbon NMR characterization of the polymorphs of roxifiban
Author(s)
Vickery, R.D., Nemeth, G.A., Maurin, M.B., 
Journal
Journal of Pharmaceutical and Biomedical Analysis 
Vol. 30, No. 1, pages 125-129 (2002) 
ISSN
0731-7085 
Publisher
Elsevier 
Abstract
Roxifiban, an experimental antithrombotic prodrug, exists as crystalline forms I and II. A quantitative solid-state nuclear magnetic resonance (NMR) method was developed to characterize the two polymorphs of roxifiban. The differences in the NMR spectra of the polymorphs were utilized in analyses of physical blends of the pure crystalline forms to establish a calibration curve. A detection limit of 9% form II in form I was determined from analysis of a 10% form II blend. Solid-state NMR was a valuable technique to quantify the polymorphic purity of roxifiban where other techniques such as differential scanning calorimetry (DSC) could not be used for this purpose.


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celan
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原文由 ausky 发表:
请教各位老师,谢谢!

Solid-state carbon NMR 可以定量,请看下面的文章.该文研究的是一种药物roxifiban,我把它的结构也帖出来供参考.
Title
Solid-state carbon NMR characterization of the polymorphs of roxifiban
Author(s)
Vickery, R.D., Nemeth, G.A., Maurin, M.B., 
Journal
Journal of Pharmaceutical and Biomedical Analysis 
Vol. 30, No. 1, pages 125-129 (2002) 
ISSN
0731-7085 
Publisher
Elsevier 
Abstract
Roxifiban, an experimental antithrombotic prodrug, exists as crystalline forms I and II. A quantitative solid-state nuclear magnetic resonance (NMR) method was developed to characterize the two polymorphs of roxifiban. The differences in the NMR spectra of the polymorphs were utilized in analyses of physical blends of the pure crystalline forms to establish a calibration curve. A detection limit of 9% form II in form I was determined from analysis of a 10% form II blend. Solid-state NMR was a valuable technique to quantify the polymorphic purity of roxifiban where other techniques such as differential scanning calorimetry (DSC) could not be used for this purpose.


ausky
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汪老师,您的资料我已经看过了,非常感谢!该论文里讨论的好像是共混物中两种不同成分的定量鉴定,如果是同一种化合物中不同化学环境的碳的定量,可不可以用CP/MAS来测试,还是有别的方法呢?
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