title: Determination of Oversulphated Chondroitin Sulphate and Dermatan Sulphate in unfractionated heparin by (1)H-NMR - Collaborative study for quantification and analytical determination of LoD.
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.
authors.affiliation: Medical Products Agency, Uppsala, Sweden. ian.mcewen@mpa.se
authors.forename: I
authors.initials: I
authors.lastname: McEwen
authors.forename: B
authors.initials: B
authors.lastname: Mulloy
authors.forename: E
authors.initials: E
authors.lastname: Hellwig
authors.forename: L
authors.initials: L
authors.lastname: Kozerski
authors.forename: T
authors.initials: T
authors.lastname: Beyer
authors.forename: U
authors.initials: U
authors.lastname: Holzgrabe
authors.forename: R
authors.initials: R
authors.lastname: Wanko
authors.forename: J-M
authors.initials: JM
authors.lastname: Spieser
authors.forename: A
authors.initials: A
authors.lastname: Rodomonte
mesh_terms: D002118:Calcium / Q000032:analysis / Q000737:chemistry; D002809:Chondroitin Sulfates / Q000032:analysis* / Q000737:chemistry; D003871:Dermatan Sulfate / Q000032:analysis* / Q000737:chemistry; D003903:Deuterium / Q000737:chemistry; D004340:Drug Contamination; D005060:Europe; D006493:Heparin / Q000032:analysis* / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation / Q000379:methods*; D015394:Molecular Structure; D010602:Pharmacopoeias as Topic; D011134:Polysaccharides / Q000032:analysis / Q000737:chemistry; D012964:Sodium / Q000032:analysis / Q000737:chemistry; D012996:Solutions / Q000032:analysis / Q000737:chemistry; D014867:Water / Q000737:chemistry
chemical_list: D011134:Polysaccharides; D012996:Solutions; D014867:Water; D003871:Dermatan Sulfate; D006493:Heparin; D002809:Chondroitin Sulfates; D012964:Sodium; D003903:Deuterium; D002118:Calcium