Scientific Publications by FDA Staff

Anal Biochem 2015 Dec 1;490:52-4

Synthesis and detection of N-sulfonated oversulfated chondroitin sulfate in marketplace heparin.

Mans DJ, Ye H, Dunn JD, Kolinski RE, Long DS, Phatak NL, Ghasriani H, Buhse LF, Kauffman JF, Keire DA

NSOSCS, recently reported as a potential threat to the heparin supply, has been prepared along with its intermediate derivatives. All compounds were spiked into marketplace heparin and subjected to USP identification assays for heparin (1H NMR, chromatographic identity, %galactosamine (%GalN), anti-factor IIa potency and anti-factor Xa:IIa ratio). The FDA strong-anionic exchange high-performance liquid chromatography method resolved NS-OSCS from heparin and OSCS and had a limit of detection of 0.26% (w/w) NS-OSCS. The %GalN test was sensitive to the presence of NS-OSCS in heparin. Therefore, current USP heparin monograph tests (i.e. SAX-HPLC and %GalN) detect the presence of NS-OSCS in heparin.