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肝素与硫酸皮肤素及其他糖胺聚糖混合物的核磁共振谱。硫酸软骨素的二维谱。

Nuclear magnetic resonance spectra of heparin in admixture with dermatan sulfate and other glycosaminoglycans. 2-D spectra of the chondroitin sulfates.

作者信息

Holme K R, Perlin A S

机构信息

Department of Chemistry, McGill University, Montreal, Canada.

出版信息

Carbohydr Res. 1989 Mar 15;186(2):301-12. doi: 10.1016/0008-6215(89)84044-3.

Abstract

Characteristics of the 1H-n.m.r. spectra of heparin admixed with other glycosaminoglycans are described with respect to the identification of the latter as possible contaminants of pharmaceutical heparins. Chemical shift differences are sufficiently large, particularly with the aid of resolution enhancement, to allow for the detection of dermatan sulfate, chondroitin 4- or 6-sulfate, hyaluronic acid, or heparan sulfate as a minor constituent in the presence of heparin. The acetamidomethyl resonance region (delta 1.95-2.15) is especially useful in this context, both for identification and quantitative estimation. Whereas dermatan sulfate is a common contaminant of pharmaceutical heparin preparations, in some instances comprising 10-15 percent of the polymer mixture, the other glycosaminoglycans, by contrast, were not detected in such preparations. Two-dimensional heterocorrelation and homo-correlation n.m.r. experiments have provided 1H- and 13C-chemical shift data that complete or verify (or both) previous information available for heparin, dermatan sulfate, and chondroitin 4- and 6-sulfates (chondroitins A and C).

摘要

关于将其他糖胺聚糖鉴定为药用肝素可能的污染物,描述了与肝素混合的1H-核磁共振谱的特征。化学位移差异足够大,特别是借助分辨率增强,能够在肝素存在的情况下检测出硫酸皮肤素、硫酸软骨素4-或6-硫酸盐、透明质酸或硫酸乙酰肝素作为次要成分。在这种情况下,乙酰氨基甲基共振区域(δ1.95 - 2.15)对于鉴定和定量估计特别有用。虽然硫酸皮肤素是药用肝素制剂的常见污染物,在某些情况下占聚合物混合物的10 - 15%,但相比之下,在这类制剂中未检测到其他糖胺聚糖。二维异核相关和同核相关核磁共振实验提供了1H和13C化学位移数据,这些数据完善或验证了(或两者兼有)先前可得的关于肝素、硫酸皮肤素以及硫酸软骨素4-和6-硫酸盐(软骨素A和C)的信息。

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