Determination of fexofenadine in human plasma using 96-well solid phase extraction and HPLC with tandem mass spectrometric detection

2004 ◽  
Vol 35 (4) ◽  
pp. 837-846 ◽  
Author(s):  
I. Fu ◽  
E.J. Woolf ◽  
B.K. Matuszewski
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Tandem Mass Spectrometric

scholarly journals Development and Validation of Salbutamol, Bromhexine, Ambroxol and Guauaifenesin Determination in Human Plasma by HPLC-MS/MS Method

2019 ◽  
Vol 8 (4) ◽  
pp. 61-74
Author(s):  
T. N. Komarov ◽  
D. S. Bogdanova ◽  
O. A. Miskiv ◽  
A. V. Aleshina ◽  
I. E. Shohin ◽  
...  
Keyword(s):  
Human Plasma ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Tandem Mass Spectrometric ◽  
Development And Validation

Introduction. Multicomponent oral drugs containing salbutamol, bromhexine, ambroxol and guaifenesin have a mucolytic, expectorant and bronchodilator effect. The development method for determination substances in biological fluids is a main procedure for performing the analytical part of pharmacokinetic studies and bioequivalence studies of multicomponent drugs. There is no published data of the determination of bromhexine, ambroxol and guaifenesin, but there a lot of published methods for divided determination analytes in a biological fluid. This study presents the development and validation of a method of the determination of salbutamol, bromhexine, ambroxol and guaifenesin in human blood plasma by high performance liquid chromatography with tandem mass spectrometric detection. A sample preparation was perfomed by solid-phase extraction. Deuterated derivatives were used as internal standards.Aim. The aim of the study is to develop a method for the quantitative determination of salbutamol, bromhexine, ambroxol and guaifenesin in human plasma by HPLC with tandem mass spectrometric detection for performing the analytical part of pharmacokinetic studies.Materials and methods. Determination of salbutamol, bromhexine, ambroxol and guaifenesin in human plasma by HPLC with tandem mass spectrometric detection. A sample was prepared using solid-phase extraction.Results and discussion. The method was validated by next validation parameters: selectivity, matrix effect, calibration curve, accuracy, precision, limit of quantification, carry-over and stability.Conclusion. The method of the determination of salbutamol, bromhexine, ambroxol and guaifenesin in human plasma was developed and validated by HPLC-MS/MS. The analytical range of the was 0.1–20 ng/mL in plasma for salbutamol, 0.25–25 ng/mL in plasma for bromhexine, 0.075–3 ng/mL in plasma for ambroxol, and 10–2000 ng/mL in plasma for guaifenesin. Method could be applied to determination of salbutamol, bromhexine, ambroxol and guaifenesin in plasma for PK and BE studies. 

scholarly journals Plasma Free Metanephrine Measurement Using Automated Online Solid-Phase Extraction HPLC–Tandem Mass Spectrometry

2007 ◽  
Vol 53 (9) ◽  
pp. 1684-1693 ◽  
Author(s):  
Wilhelmina HA de Jong ◽  
Kendon S Graham ◽  
Jan C van der Molen ◽  
Thera P Links ◽  
Michael R Morris ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Analytical Sensitivity ◽  
Automated Method ◽  
Online Solid Phase Extraction ◽  
Tandem Mass Spectrometric

Abstract Background: Quantification of plasma free metanephrine (MN) and normetanephrine (NMN) is considered to be the most accurate test for the clinical chemical diagnosis of pheochromocytoma and follow-up of pheochromocytoma patients. Current methods involve laborious, time-consuming, offline sample preparation, coupled with relatively nonspecific detection. Our aim was to develop a rapid, sensitive, and highly selective automated method for plasma free MNs in the nanomole per liter range. Methods: We used online solid-phase extraction coupled with HPLC-tandem mass spectrometric detection (XLC-MS/MS). Fifty microliters plasma equivalent was prepurified by automated online solid-phase extraction, using weak cation exchange cartridges. Chromatographic separation of the analytes and deuterated analogs was achieved by hydrophilic interaction chromatography. Mass spectrometric detection was performed in the multiple reaction monitoring mode using a quadrupole tandem mass spectrometer in positive electrospray ionization mode. Results: Total run-time including sample cleanup was 8 min. Intra- and interassay analytical variation (CV) varied from 2.0% to 4.7% and 1.6% to 13.5%, respectively, whereas biological intra- and interday variation ranged from 9.4% to 45.0% and 8.4% to 23.2%. Linearity in the 0 to 20 nmol/L calibration range was excellent (R2 > 0.99). For all compounds, recoveries ranged from 74.5% to 99.6%, and detection limits were <0.10 nmol/L. Reference intervals for 120 healthy adults were 0.07 to 0.33 nmol/L (MN), 0.23 to 1.07 nmol/L (NMN), and <0.17 nmol/L (3-methoxytyramine). Conclusions: This automated high-throughput XLC-MS/MS method for the measurement of plasma free MNs is precise and linear, with short analysis time and low variable costs. The method is attractive for routine diagnosis of pheochromocytoma because of its high analytical sensitivity, the analytical power of MS/MS, and the high diagnostic accuracy of free MNs.

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