Determination of Oversulphated Chondroitin Sulphate and Dermatan Sulphate in unfractionated heparin by (1)H-NMR - Collaborative study for quantification and analytical determination of LoD.
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.
McEwen
I
I
Medical Products Agency, Uppsala, Sweden. ian.mcewen@mpa.se
Mulloy
B
B
Hellwig
E
E
Kozerski
L
L
Beyer
T
T
Holzgrabe
U
U
Wanko
R
R
Spieser
J-M
JM
Rodomonte
A
A
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
D011134:Polysaccharides; D012996:Solutions; D014867:Water; D003871:Dermatan Sulfate; D006493:Heparin; D002809:Chondroitin Sulfates; D012964:Sodium; D003903:Deuterium; D002118:Calcium