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1.
J Chromatogr B Analyt Technol Biomed Life Sci ; 852(1-2): 115-21, 2007 Jun 01.
Article in English | MEDLINE | ID: mdl-17296337

ABSTRACT

A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the estimation of rivastigmine in human plasma. Rivastigmine was extracted from human plasma by using solid-phase extraction technique. Zolpidem was used as the internal standard. A Betabasic-8 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 251.20-->206.10, 86.20 for rivastigmine and m/z 308.10-->235.10 for zolpidem. The method involves a rapid solid-phase extraction from plasma, simple isocratic chromatographic conditions and mass spectrometric detection that enables detection at sub-nanogram levels. The proposed method has been validated for a linear range of 0.2-20.0 ng/ml with a correlation coefficient > or =0.9988. The intra-run and inter-run precision and accuracy were within 10.0%. The overall recoveries for rivastigmine and zolpidem were 86.28% and 87.57%, respectively. The total run time was 2.0 min. The developed method was applied for the determination of the pharmacokinetic parameters of rivastigmine following a single oral administration of a 3 mg rivastigmine capsule in 20 healthy male volunteers.


Subject(s)
Cholinesterase Inhibitors/blood , Phenylcarbamates/blood , Tandem Mass Spectrometry/methods , Administration, Oral , Cholinesterase Inhibitors/pharmacokinetics , Humans , Male , Phenylcarbamates/pharmacokinetics , Reference Standards , Reproducibility of Results , Rivastigmine , Sensitivity and Specificity
2.
J Chromatogr B Analyt Technol Biomed Life Sci ; 852(1-2): 374-81, 2007 Jun 01.
Article in English | MEDLINE | ID: mdl-17324642

ABSTRACT

A high throughput and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the estimation of bisoprolol in human plasma using multiplexing technique (two HPLC units connected to one MS). Bisoprolol was extracted from human plasma using solid-phase extraction technique using metoprolol as internal standard. A Betabasic 8 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 326.2-->116.1 for bisoprolol and m/z 268.2-->191.0 for metoprolol. The method involves a simple multiplexing, rapid solid-phase extraction, simple isocratic chromatography conditions and mass spectrometric detection which enable detection at sub-nanogram levels. The proposed method has been validated for a linear range of 0.5-70.0 ng/mL with correlation coefficient > or =0.9991. The precision and accuracy were within 10% for intra-HPLC runs and inter-HPLC runs. The overall recoveries for bisoprolol and metoprolol were 93.89% and 77.65%, respectively. Total MS run time was 0.90 min only. The developed method was applied for the determination of pharmacokinetic parameters of bisoprolol following a single oral administration of a 10mg bisoprolol tablet in 18 healthy male volunteers.


Subject(s)
Adrenergic beta-Antagonists/blood , Bisoprolol/blood , Chromatography, High Pressure Liquid/methods , Tandem Mass Spectrometry/methods , Humans , Reference Standards , Reproducibility of Results , Sensitivity and Specificity
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