Automated Post-Column Sample Manipulation Prior to Detection in Liquid Chromatography: A Review of Pharmaceutical and Bioanalytical Applications

2019 ◽  
Vol 15 (7) ◽  
pp. 759-775 ◽  
Author(s):  
Natalia Manousi ◽  
Constantinos K. Zacharis
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Biomedical Applications ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Ionization Efficiency ◽  
Ion Suppression ◽  
On Line ◽  
Bioanalytical Applications

: Automated post-column sample manipulation is undoubtedly one of the most challenging approaches in liquid chromatography for the improvement of method selectivity and sensitivity. With the post-column analyte derivatization being the most-abundant approach approach of this category, other strategies typically comprise post-column infusion of internal standard or other reagents prior to mass spectrometric detection to enhance the ionization efficiency of the analyte or to compensate the ion suppression/enhancement. : In this review, on-line post column methodologies focused on the quality control of pharmaceuticals and biomedical applications will be presented and discussed. Emphasis will be given on the automation capabilities of such systems.

scholarly journals Enantioselective Determination Of S- And R-Isomers Of Ibuprofen In Plasma By Ultra-Performance Liquid Chromatography – Tandem Mass Spectrometry

2020 ◽  
Vol 15 (1) ◽  
pp. 40-46
Author(s):  
V.O. DOROSCHUK ◽  
V.Ye. Sabko ◽  
O.V. Ivashko ◽  
L.O. POPOVA ◽  
A.S. Shalamay
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Tandem Mass ◽  
Ibuprofen Enantiomers ◽  
Tandem Mass Spectrometric

A new method of enantioselective determination of S- and R-isomers of ibuprofen in human plasma by ultraperformance liquid chromatography with tandem mass spectrometric detection using solid-phase extraction was developed. For enantioselective separation of ibuprofen isomers, a LUX Cellulose-3 chiral chromatographic column was used. Complete separation of the enathiomer peaks is achieved in the isocratic elution conditions with a mobile phase ratio of 0.05 % formic acid solution (%): methanol (%) = 30 : 70 (v/v) and a flow rate of 0.2 mL/min. The mass spectrometric detection was performed at negative ionization mode with multiple reaction monitoring, using the transitions at 205.13 > 161.14 Da and 208.09 > 164.03 Da for ibuprofen enantiomers and deuterated ibuprofen (internal standard), respectively. The method validation included the evaluation of the selectivity, linearity, lower limit of quantification (LLOQ), within-run and between-run precision and accuracy. The LLOQ for the two enantiomers was 100 ng/mL in plasma. The calibration curves showed good linearity of each enantiomers in the ranges from 100 to 60000 ng/mL. The method was successfully applied to a pharmacokinetic study of ibuprofen enantiomers in human plasma.

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