TY - JOUR T1 - Characterization of currently marketed heparin products: reversed-phase ion-pairing liquid chromatography mass spectrometry of heparin digests. AU - Brustkern,Adam M, AU - Buhse,Lucinda F, AU - Nasr,Moheb, AU - Al-Hakim,Ali, AU - Keire,David A, Y1 - 2010/11/11/ PY - 2010/11/13/entrez PY - 2010/11/13/pubmed PY - 2011/3/17/medline SP - 9865 EP - 70 JF - Analytical chemistry JO - Anal Chem VL - 82 IS - 23 N2 - Here we report results from the analyses by enzymatic digestion and reversed-phase ion-pairing liquid chromatography mass spectrometry (RPIP-LC-MS) of active pharmaceutical ingredient (API) unfractionated heparins (UFHs) from six different manufacturers and one USP standard sample. We employed a reverse phase ion-pairing chromatography method using a C(18) column and hexylamine as the ion-pairing reagent with acetonitrile gradient elution to separate disaccharides generated from the digestion of the heparins by lyase I and III (E.C. 4.2.2.7 and 4.2.2.8) before introduction into an ion-trap mass spectrometer by an electrospray ionization (ESI) interface. Extracted ion chromatograms (EICs) were used to determine the relative abundance of the disaccharides by mass spectrometry. Eight disaccharides were observed and a similar composition profile was observed from digests of 20 UFH samples. The compositional profile determined from these experiments provides a measure of the norm and range of variation in "good" heparin to which future preparations can be compared. Furthermore, the profile obtained in the RPIP-LC-MS assay is sensitive to the presence of the contaminant, oversulfated chondroitin sulfate A (OSCS), in heparin. SN - 1520-6882 UR - https://www.unboundmedicine.com/medline/citation/21069966/Characterization_of_currently_marketed_heparin_products:_reversed_phase_ion_pairing_liquid_chromatography_mass_spectrometry_of_heparin_digests_ L2 - https://doi.org/10.1021/ac102301j DB - PRIME DP - Unbound Medicine ER -