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Simultaneous Quantification of Mesalamine and Its Metabolite N-Acetyl Mesalamine in Human Plasma by LC-MS/MS and Its Application to a Bioequivalence Study

Kanchanamala Kanala, Nagiat T. Hwisa, Babu Rao Chandu, Fathi H. Assaleh, K. Mukkanti, Prakash Katakam, Bala Sekhara Reddy Challa

Journal of Pharmaceutical Research International · pp. 1568–1590 · Published 21 Jun 2014

10.9734/BJPR/2014/5350

Abstract

Liquid chromatography–tandem mass spectrometry (LC–MS/MS) was used for simultaneous quantification of mesalamine and its metabolite N-acetyl mesalamine in human plasma with N-acetyl mesalamine D3 as an internal standard (IS). Chromatographic separation was performed on a Thermo, HyPURITY C18 (150 x 4.6 mm, 5 m) column with an isocratic mobile phase composed of 10 mM ammonium acetate and methanol in the ratio of 85:15 (%v/v), at the flowrate of 0.6 mL/min. The drug, metabolite and internal standard were extracted by liquid-liquid extraction. The method was validated over a linear concentration range of 2-1500 ng/mL for mesalamine and 10-2000 ng/ml for N-acetyl mesalamine, which demonstrated intra and inter-day precision ranging from 1.60 to 8.63% and 2.14 to 8.67% for mesalamine and 0.99 to 5.67% and 1.72 to 4.89% for N-acetyl mesalamine respectively. Similarly, the intra- and inter-day accuracy varied from 102.70 to 105.48% and 100.64 to 103.87% for mesalamine, 99.64 to 106.22% and 100.71 to 104.27% for N-acetyl mesalamine respectively. Both analytes were found to be stable throughout freeze–thawing cycles, bench top and postoperative stability studies. The method was successfully applied to support a bioequivalance study of healthy subjects.

Mesalamine N-Acetyl mesalamine LC/MS/MS bioequivalence pharmacokinetics

References (34)

  1. 1 High-performance liquid-chromatographic determination of 5-aminosalicylic acid and its metabolites in blood plasma [DOI]
  2. 2 Development and validation of a HPLC-ESI-MS/MS method for the determination of 5-aminosalicylic acid and its major metabolite N-acetyl-5-aminosalicylic acid in human plasma [DOI]
  3. 3 Determination of 5-aminosalicylic acid in pharmaceutical formulation by differential pulse voltammetry [DOI]
  4. 4 Determination of sulphasalazine and its main metabolite sulphapyridine and 5-aminosalicylic acid in human plasma by liquid chromatography/tandem mass spectrometry and its application to a pharmacokinetic study [DOI]
  5. 5 Quantitative HPLC analysis of mebeverine, mesalazine, sulphasalazine and dispersible aspirin stored in a Venalink monitored dosage system with co-prescribed medicines [DOI]
  6. 6 Simple method for the determination of 5-aminosalicylic and N-acetyl-5-aminosalicylic acid in rectal tissue biopsies [DOI]
  7. 7 5-Aminosalicylic Acid in a Slow-Release Preparation: Bioavailability, Plasma Level, and Excretion in Humans [DOI]
  8. 8 A validated HPLC method with electrochemical detection for simultaneous assay of 5‐aminosalicylic acid and its metabolite in human plasma [DOI]
  9. 9 Simultaneous determination of 5-aminosalicylic acid, acetyl-5-aminosalicylic acid and 2,5-dihydroxybenzoic acid in endoscopie intestinal biopsy samples in humans by high-performance liquid chromatography with electrochemical detection [DOI]
  10. 10 Validation of a LC method for the determination of 5-aminosalicylic acid and its metabolite in plasma and urine [DOI]
  11. 11 Comparative bioavailability of 5‐aminosalicylic acid from a controlled release preparation and an azo‐bond preparation [DOI]
  12. 12 Identification of reaction products between drug substances and excipients by HPLC–SPE–NMR: Ester and amide formation between citric acid and 5-aminosalicylic acid [DOI]
  13. 13 Voltammetric studies of 2-hydroxy-5-[(4-sulfophenyl)azo]benzoic acid as a novel prodrug of 5-aminosalicylic acid [DOI]
  14. 14 Absorption kinetics of 5-aminosalicylic acid in rat: influence of indomethacin-induced gastrointestinal lesions and Escherichia Coli Nissle 1917 medication.
  15. 15 The application of LC–NMR and LC–MS for the separation and rapid structure elucidation of an unknown impurity in 5-aminosalicylic acid [DOI]
  16. 16 Experimental Goettingen minipig and beagle dog as two species used in bioequivalence studies for clinical pharmacology (5-aminosalicylic acid and atenolol as model drugs).
  17. 17 LC-MS/MS and FT-IR analyses of stones from a patient with Crohn’s disease: a case report [DOI]
  18. 18 Determination of impurities in the drug 5-aminosalicylic acid by micellar electrokinetic capillary chromatography using an electrolyte pH that approaches the isoelectric point of the parent compound [DOI]
  19. 19 Assay of 5-aminosalicylate and its acetylated metabolite in biological fluids by high-performance liquid chromatography on dynamically modified silica [DOI]
  20. 20 Simplified high-performance liquid chromatographic method for 5-amino-salicylic acid in plasma and urine [DOI]
  21. 21 Pharmacokinetics of a 5‐aminosalicylic acid enteric‐coated tablet in patients with Crohn's disease or ulcerative colitis and in healthy volunteers [DOI]
  22. 22 Comparative pharmacokinetics of equimolar doses of 5‐aminosalicylate administered as oral mesalamine (Asacol) and balsalazide: a randomized, single‐dose, crossover study in healthy volunteers1 [DOI]
  23. 23 High-performance liquid chromatographic assay for the determination of 5-aminosalicylic acid and acetyl-5-aminosalicylic acid concentrations in endoscopic intestinal biopsy in humans [DOI]
  24. 24 Simple and sensitive high-performance liquid chromatographic assay for 5-aminosalicylic acid and acetyl-5-aminosalicylic acid in serum [DOI]
  25. 25 Investigation of the stability of 5-aminosalicylic acid in tablets and suppositories by high-performance liquid chromatography [DOI]
  26. 26 Chemistry, Pharmacology, Pharmacokinetics, and Clinical Applications of Mesalamine for the Treatment of Inflammatory Bowel Disease [DOI]
  27. 27 High-performance liquid chromatographic assay of 5-aminosalicylic acid and its acetylated metabolite in biological fluids using electrochemical detection [DOI]
  28. 28 Bioavailability of single and multiple doses of a new oral formulation of 5‐ASA in patients with inflammatory bowel disease and healthy volunteers [DOI]
  29. 29 Bioavailability of Single and Multiple Doses of Enteric-Coated Mesalamine and Sulphasalazine [DOI]
  30. 30 Ion-pairing high-performance liquid chromatographic method for the determination of 5-aminosalicylic acid and related impurities in bulk chemical [DOI]
  31. 31 Pharmacokinetics and safety of single and multiple doses of Asacol tablets in Japanese healthy volunteers [DOI]
  32. 32 Mono- and Biphasic Plasma Concentration-time Curves of Mesalazine from a 500 mg Suppository in Healthy Male Volunteers Controlled by the Time of Defecation before Dosing [DOI]
  33. 33 Simultaneous determination of 5-aminosalicylic acid and 5-acetylaminosalicylic acid by high-performance liquid chromatography [DOI]
  34. 34 [Study on the analysis of zinc 5-aminosalicylate and related compounds by high performance liquid chromatography].

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