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通过¹H-NMR测定未分级肝素中过度硫酸化硫酸软骨素和硫酸皮肤素 - 最低检测限定量及分析测定的协作研究

Determination of Oversulphated Chondroitin Sulphate and Dermatan Sulphate in unfractionated heparin by (1)H-NMR - Collaborative study for quantification and analytical determination of LoD.

作者信息

McEwen I, Mulloy B, Hellwig E, Kozerski L, Beyer T, Holzgrabe U, Wanko R, Spieser J-M, Rodomonte A

机构信息

Medical Products Agency, Uppsala, Sweden.

出版信息

Pharmeuropa Bio. 2008 Dec;2008(1):31-9.

Abstract

Oversulphated Chondroitin Sulphate (OSCS) and Dermatan Sulphate (DS) in unfractionated heparins can be identified by nuclear magnetic resonance spectrometry (NMR). The limit of detection (LoD) of OSCS is 0.1% relative to the heparin content. This LoD is obtained at a signal-to-noise ratio (S/N) of 2000:1 of the heparin methyl signal. Quantification is best obtained by comparing peak heights of the OSCS and heparin methyl signals. Reproducibility of less than 10% relative standard deviation (RSD) has been obtained. The accuracy of quantification was good.

摘要

未分级肝素中的过度硫酸化硫酸软骨素(OSCS)和硫酸皮肤素(DS)可通过核磁共振光谱法(NMR)进行鉴定。相对于肝素含量,OSCS的检测限(LoD)为0.1%。该检测限是在肝素甲基信号的信噪比(S/N)为2000:1时获得的。通过比较OSCS和肝素甲基信号的峰高可实现最佳定量。已获得相对标准偏差(RSD)小于10%的重现性。定量准确性良好。

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