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Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method.
Anal Chim Acta. 2008 Nov 23; 629(1-2):145-57.AC

Abstract

A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous determination of donepezil (D) and its pharmacologically active metabolite, 6-O-desmethyl donepezil (6-ODD) in human plasma is developed using galantamine as internal standard (IS). The analytes and IS were extracted from 500 microL aliquots of human plasma via solid-phase extraction (SPE) on Waters Oasis HLB cartridges. Chromatographic separation was achieved in a run time of 6.0 min on a Waters Novapak C18 (150 mm x 3.9 mm, 4 microm) column under isocratic conditions. Detection of analytes and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for D, 6-ODD and IS were at m/z 380.1-->91.2, 366.3-->91.3 and 288.2-->213.2, respectively. The method was fully validated for its selectivity, interference check, sensitivity, linearity, precision and accuracy, recovery, matrix effect, ion suppression/enhancement, cross-specificity, stability and dilution integrity. A linear dynamic range of 0.10-50.0 ng mL(-1) for D and 0.02-10.0 ng mL(-1) for 6-ODD was evaluated with mean correlation coefficient (r) of 0.9975 and 0.9985, respectively. The intra-batch and inter-batch precision (%CV, coefficient of variation) across five quality control levels was less than 7.5% for both the analytes. The method was successfully applied to a bioequivalence study of 10mg donepezil tablet formulation in 24 healthy Indian male subjects under fasting condition.

Authors+Show Affiliations

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

Pub Type(s)

Journal Article

Language

eng

PubMed ID

18940331

Citation

Patel, Bhavin N., et al. "Quantitation of Donepezil and Its Active Metabolite 6-O-desmethyl Donepezil in Human Plasma By a Selective and Sensitive Liquid Chromatography-tandem Mass Spectrometric Method." Analytica Chimica Acta, vol. 629, no. 1-2, 2008, pp. 145-57.
Patel BN, Sharma N, Sanyal M, et al. Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method. Anal Chim Acta. 2008;629(1-2):145-57.
Patel, B. N., Sharma, N., Sanyal, M., & Shrivastav, P. S. (2008). Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method. Analytica Chimica Acta, 629(1-2), 145-57. https://doi.org/10.1016/j.aca.2008.09.048
Patel BN, et al. Quantitation of Donepezil and Its Active Metabolite 6-O-desmethyl Donepezil in Human Plasma By a Selective and Sensitive Liquid Chromatography-tandem Mass Spectrometric Method. Anal Chim Acta. 2008 Nov 23;629(1-2):145-57. PubMed PMID: 18940331.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method. AU - Patel,Bhavin N, AU - Sharma,Naveen, AU - Sanyal,Mallika, AU - Shrivastav,Pranav S, Y1 - 2008/10/01/ PY - 2008/06/21/received PY - 2008/09/18/revised PY - 2008/09/19/accepted PY - 2008/10/23/pubmed PY - 2009/2/12/medline PY - 2008/10/23/entrez SP - 145 EP - 57 JF - Analytica chimica acta JO - Anal Chim Acta VL - 629 IS - 1-2 N2 - A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous determination of donepezil (D) and its pharmacologically active metabolite, 6-O-desmethyl donepezil (6-ODD) in human plasma is developed using galantamine as internal standard (IS). The analytes and IS were extracted from 500 microL aliquots of human plasma via solid-phase extraction (SPE) on Waters Oasis HLB cartridges. Chromatographic separation was achieved in a run time of 6.0 min on a Waters Novapak C18 (150 mm x 3.9 mm, 4 microm) column under isocratic conditions. Detection of analytes and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for D, 6-ODD and IS were at m/z 380.1-->91.2, 366.3-->91.3 and 288.2-->213.2, respectively. The method was fully validated for its selectivity, interference check, sensitivity, linearity, precision and accuracy, recovery, matrix effect, ion suppression/enhancement, cross-specificity, stability and dilution integrity. A linear dynamic range of 0.10-50.0 ng mL(-1) for D and 0.02-10.0 ng mL(-1) for 6-ODD was evaluated with mean correlation coefficient (r) of 0.9975 and 0.9985, respectively. The intra-batch and inter-batch precision (%CV, coefficient of variation) across five quality control levels was less than 7.5% for both the analytes. The method was successfully applied to a bioequivalence study of 10mg donepezil tablet formulation in 24 healthy Indian male subjects under fasting condition. SN - 1873-4324 UR - https://www.unboundmedicine.com/medline/citation/18940331/Quantitation_of_donepezil_and_its_active_metabolite_6_O_desmethyl_donepezil_in_human_plasma_by_a_selective_and_sensitive_liquid_chromatography_tandem_mass_spectrometric_method_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0003-2670(08)01698-X DB - PRIME DP - Unbound Medicine ER -