Liquid chromatography and tandem mass spectrometry method for the quantitative determination of saxagliptin and its major pharmacologically active 5-monohydroxy metabolite in human plasma: Method validation and overcoming specific and non-specific binding at low concentrations

Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences

Volumn 889-890, Issue , 2012, Pages 77-86

  Xu, Xiaohui Sophia ^a   Demers, Roger ^b   Gu, Huidong ^a   Christopher, Lisa J ^a   Su, Hong ^a   Cojocaru, Laura ^b   Boulton, David W ^a   Kirby, Mark ^a   Stouffer, Bruce ^a   Humphreys, William G ^a   Arnold, Mark E ^a  

^a BRISTOL MYERS SQUIBB   (United States)

^b Tandem Labs   (United States)

Author keywords

5 Hydroxy saxagliptin metabolite; Antidiabetic agent; BMS 477118; Cross validation; Diastereomer; Dipeptide peptidase; DPP4; Human plasma; LC MS MS; Liquid chromatography tandem mass spectrometry; Onglyza ; Protein precipitation; Saxagliptin

Indexed keywords

ANTIDIABETIC AGENTS; BMS-477118; CROSS VALIDATION; DIASTEREOMERS; DIPEPTIDE-PEPTIDASE; DPP4; HUMAN PLASMAS; LC-MS/MS; LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY; PROTEIN PRECIPITATION; SAXAGLIPTIN;

ACETONITRILE; BIOMOLECULES; CHROMATOGRAPHY; ISOMERS; MASS SPECTROMETRY; METABOLISM; METABOLITES; PLASMA (HUMAN);

HIGH PRESSURE LIQUID CHROMATOGRAPHY;

3 [(3 CHOLAMIDOPROPYL)DIMETHYLAMMONIO] 1 PROPANESULFONIC ACID; 5 HYDROXY SAXAGLIPTIN; ACETONITRILE; DRUG METABOLITE; METFORMIN; SAXAGLIPTIN; UNCLASSIFIED DRUG;

ARTICLE; DRUG BLOOD LEVEL; DRUG DETERMINATION; DRUG HALF LIFE; DRUG STABILITY; DRUG STRUCTURE; HIGH PERFORMANCE LIQUID CHROMATOGRAPHY; HUMAN; LIQUID CHROMATOGRAPHY; PRIORITY JOURNAL; TANDEM MASS SPECTROMETRY;

ADAMANTANE; CHROMATOGRAPHY, LIQUID; DIPEPTIDES; DRUG STABILITY; HUMANS; REPRODUCIBILITY OF RESULTS; SENSITIVITY AND SPECIFICITY; STEREOISOMERISM; TANDEM MASS SPECTROMETRY;

EID: 84862822679     PISSN: 15700232     EISSN: 1873376X     Source Type: Journal    
DOI: 10.1016/j.jchromb.2012.01.033     Document Type: Article

References (14)

1. United States Prescribing Information for Onglyza™ (Saxagliptin) 2011, Bristol-Myers Squibb Company and AstraZeneca Pharmaceuticals.
2. Kirby M., Yu D.M., O'Connor S., Gorrell M.D. Clin. Sci. (Lond.) 2010, 118:31.
3. D.W. Boulton, M. Geraldes, Presented as poster (0606-P) at the American Diabetic Association's 67th Annual Scientific Session, 2007.
4. Augeri D.J., Robl J.A., Betebenner D.A., Magnin D.R., Khanna A., Robertson J.G., Wang A., Simpkins L.M., Taunk P., Huang Q., Han S.P., Abboa-Offei B., Cap M., Xin L., Tao L., Tozzo E., Welzel G.E., Egan D.M., Marcinkeviciene J., Chang S.Y., Biller S.A., Kirby M.S., Parker R.A., Hamann L.G. J. Med. Chem. 2005, 48:5025.
5. Fura A., Khanna A., Vyas V., Koplowitz B., Chang S.Y., Caporuscio C., Boulton D.W., Christopher L.J., Chadwick K.D., Hamann L.G., Humphreys W.G., Kirby M. Drug Metab. Dispos. 2009, 37:1164.
6. Karyekar C., Donovan M., Allen E., Fleming D., Ravichandran S., Chen R. Postgrad. Med. 2011, 123:63.
7. Boulton D.W., Li L., Frevert E.U., Tang A., Castaneda L., Vachharajani N.N., Kornhauser D.M., Patel C.G. Clin. Pharmacokinet. 2011, 50:253.
8. Patel C.G., Kornhauser D., Vachharajani N., Komoroski B., Brenner E., Handschuh del Corral M., Li L., Boulton D.W. Diabetes Obes. Metab. 2011, 13:604.
9. Food and Drug Administration, US Department of Health and Human Services Guidance for Industry: Bioanalytical Method Validation 2001.
10. Viswanathan C.T., Bansal S., Booth B., DeStefano A.J., Rose M.J., Sailstad J., Shah V.P., Skelly J.P., Swann P.G., Weiner R. Pharm. Res. 2007, 24:1962.
11. Christopher L.J., Su H., Barros A., Wang L., Cao K., Bonacorsi S., Iyer R.A., Humphreys W.G. Drug Metab. Rev. 2009, 41(s3):1.
12. Wsól V., Skálová L., Szotáková B. Curr. Drug Metab. 2004, 5:517.
13. H. Su, L.J. Christopher, R.A. Iyer, S. Bonacorsi, K. Cao, D. Boulton, W.G. Humphreys, Poster 236 at 2011 ISSX Annual Meeting, 2011.
14. Durinx C., Lambeir A.M., Bosmans E., Falmagne J.B., Berghmans R., Haemers A., Scharpé S., De Meester I. Eur. J. Biochem. 2000, 267:5608.