Quality assessment of unfractionated heparin using 1H nuclear magnetic resonance spectroscopy.

Abstract:

:Due to problems, especially anaphylactoid reactions, raised by impure unfractionated heparin the quality assessment of heparin has to be reconsidered. Neither the USP nor the European Pharmacopoeia are able to guarantee the purity of heparin, i.e., the limitation of oversulfated chondroitin sulfate (OSCS) which was found to be the reason for the allergic adverse effects. In the first run the regulatory authorities ask for 1H NMR spectroscopic and capillary electrophoretic measurements in order to characterize the impurity profile of heparin. Using an optimized 1H NMR method the limit of detection for OSCS was found to be 0.1%. In addition, it is possible to reliably quantify both OSCS and dermatan sulfate (DS), the latter being an indicator of poor purification of the unfractionated heparin. Screening of more than 100 heparin samples collected from international markets revealed a high number of samples containing substantial amounts of DS and a number of samples containing OSCS in an amount higher than 0.1%.

journal_name

J Pharm Biomed Anal

authors

Beyer T,Diehl B,Randel G,Humpfer E,Schäfer H,Spraul M,Schollmayer C,Holzgrabe U

doi

10.1016/j.jpba.2008.06.014

subject

Has Abstract

pub_date

2008-09-10 00:00:00

pages

13-9

issue

1

eissn

0731-7085

issn

1873-264X

pii

S0731-7085(08)00360-9

journal_volume

48

pub_type

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