Tags

Type your tag names separated by a space and hit enter

Liquid chromatography/electrospray ionization tandem mass spectrometry validated method for the simultaneous quantification of sibutramine and its primary and secondary amine metabolites in human plasma and its application to a bioequivalence study.
Rapid Commun Mass Spectrom. 2006; 20(23):3509-21.RC

Abstract

A high-throughput and sensitive bioanalytical method using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) has been developed for the estimation of sibutramine and its two metabolites (M1 and M2). The extraction of sibutramine, its metabolites and imipramine (internal standard (IS)) from the plasma involved treatment with phosphoric acid followed by solid-phase extraction (SPE) using a hydrophilic-lipophilic balanced HLB cartridge. The SPE eluate without drying and reconstitution was analyzed by LC/MS/MS, equipped with a with turbo ion spray (TIS) source, operating in the positive and multiple reaction monitoring (MRM) acquisition mode. Sample preparation by this method yielded extremely clean extracts with quantitative and consistent mean recoveries; 95.12% for sibutramine, 92.74% for M1, 95.97% for M2 and 96.60% for the IS. The total chromatographic run time was 3.0 min with retention times of 2.51, 2.13, 2.09 min for sibutramine, M1, M2 and imipramine, respectively. The developed method was validated in human plasma matrix, with a sensitivity of 0.1 ng/mL (coefficient of variance (CV), 2.07%) for sibutramine, 0.1 ng/mL (CV, 3.59%) for M1 and 0.2 ng/mL (CV, 4.93%) for M2. Validation of the method for its accuracy, precision, recovery, matrix effect and stability was carried out especially with regard to real subject sample analysis. The response was linear over the dynamic range 0.1 to 8.0 ng/mL for sibutramine and M1, and 0.2 to 16.0 ng/mL for M2 with correlation coefficients of r > or = 0.9959 (sibutramine), 0.9935 (M1) and 0.9943 (M2). The method was successfully applied for bioequivalence studies in 40 human subjects with 15 mg capsule formulations.

Authors+Show Affiliations

Department of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380 009, India.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article
Validation Study

Language

eng

PubMed ID

17072906

Citation

Jain, Deepak S., et al. "Liquid Chromatography/electrospray Ionization Tandem Mass Spectrometry Validated Method for the Simultaneous Quantification of Sibutramine and Its Primary and Secondary Amine Metabolites in Human Plasma and Its Application to a Bioequivalence Study." Rapid Communications in Mass Spectrometry : RCM, vol. 20, no. 23, 2006, pp. 3509-21.
Jain DS, Subbaiah G, Sanyal M, et al. Liquid chromatography/electrospray ionization tandem mass spectrometry validated method for the simultaneous quantification of sibutramine and its primary and secondary amine metabolites in human plasma and its application to a bioequivalence study. Rapid Commun Mass Spectrom. 2006;20(23):3509-21.
Jain, D. S., Subbaiah, G., Sanyal, M., Shrivastav, P. S., Pal, U., Ghataliya, S., Kakad, A., Patel, H., & Shah, S. (2006). Liquid chromatography/electrospray ionization tandem mass spectrometry validated method for the simultaneous quantification of sibutramine and its primary and secondary amine metabolites in human plasma and its application to a bioequivalence study. Rapid Communications in Mass Spectrometry : RCM, 20(23), 3509-21.
Jain DS, et al. Liquid Chromatography/electrospray Ionization Tandem Mass Spectrometry Validated Method for the Simultaneous Quantification of Sibutramine and Its Primary and Secondary Amine Metabolites in Human Plasma and Its Application to a Bioequivalence Study. Rapid Commun Mass Spectrom. 2006;20(23):3509-21. PubMed PMID: 17072906.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Liquid chromatography/electrospray ionization tandem mass spectrometry validated method for the simultaneous quantification of sibutramine and its primary and secondary amine metabolites in human plasma and its application to a bioequivalence study. AU - Jain,Deepak S, AU - Subbaiah,Gunta, AU - Sanyal,Mallika, AU - Shrivastav,Pranav S, AU - Pal,Usha, AU - Ghataliya,Shailesh, AU - Kakad,Abhijeet, AU - Patel,Heena, AU - Shah,Sapna, PY - 2006/10/31/pubmed PY - 2007/1/12/medline PY - 2006/10/31/entrez SP - 3509 EP - 21 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 20 IS - 23 N2 - A high-throughput and sensitive bioanalytical method using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) has been developed for the estimation of sibutramine and its two metabolites (M1 and M2). The extraction of sibutramine, its metabolites and imipramine (internal standard (IS)) from the plasma involved treatment with phosphoric acid followed by solid-phase extraction (SPE) using a hydrophilic-lipophilic balanced HLB cartridge. The SPE eluate without drying and reconstitution was analyzed by LC/MS/MS, equipped with a with turbo ion spray (TIS) source, operating in the positive and multiple reaction monitoring (MRM) acquisition mode. Sample preparation by this method yielded extremely clean extracts with quantitative and consistent mean recoveries; 95.12% for sibutramine, 92.74% for M1, 95.97% for M2 and 96.60% for the IS. The total chromatographic run time was 3.0 min with retention times of 2.51, 2.13, 2.09 min for sibutramine, M1, M2 and imipramine, respectively. The developed method was validated in human plasma matrix, with a sensitivity of 0.1 ng/mL (coefficient of variance (CV), 2.07%) for sibutramine, 0.1 ng/mL (CV, 3.59%) for M1 and 0.2 ng/mL (CV, 4.93%) for M2. Validation of the method for its accuracy, precision, recovery, matrix effect and stability was carried out especially with regard to real subject sample analysis. The response was linear over the dynamic range 0.1 to 8.0 ng/mL for sibutramine and M1, and 0.2 to 16.0 ng/mL for M2 with correlation coefficients of r > or = 0.9959 (sibutramine), 0.9935 (M1) and 0.9943 (M2). The method was successfully applied for bioequivalence studies in 40 human subjects with 15 mg capsule formulations. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/17072906/Liquid_chromatography/electrospray_ionization_tandem_mass_spectrometry_validated_method_for_the_simultaneous_quantification_of_sibutramine_and_its_primary_and_secondary_amine_metabolites_in_human_plasma_and_its_application_to_a_bioequivalence_study_ L2 - https://doi.org/10.1002/rcm.2760 DB - PRIME DP - Unbound Medicine ER -