Screening for library-assisted identification and fully validated quantification of 22 beta-blockers in blood plasma by liquid chromatography–mass spectrometry with atmospheric pressure chemical ionization

Abstract

A liquid chromatographic-mass spectrometric assay with atmospheric pressure chemical ionization (LC-APCI-MS) is presented for screening for, library-assisted identification (both in scan mode) and quantification (selected-ion mode) of the beta-blockers acebutolol, diacetolol, alprenolol, atenolol, betaxolol, bisoprolol, bupranolol, carazolol, carteolol, carvedilol, celiprolol, esmolol, labetalol, metoprolol, nadolol, nebivolol, oxprenolol, penbutolol, propranolol, sotalol, talinolol and timolol in blood plasma after mixed-mode (HCX) solid-phase extraction (SPE) and separation by reverse-phase liquid chromatography with gradient elution. The validation data were within the required limits. The assay was successfully applied to authentic plasma samples allowing confirmation of diagnosis of overdose situations as well as monitoring of patients' compliance.

Validation of new methods

“…This experimental design was later modified by Peters based on considerations discussed in his review article on method validation [9]. The modified design has become the basis for method validation in a series of methods published by the working group of Maurer in the last few years [44][45][46][47][48][49][50]. A detailed description of the latest version of this experimental design, which also contains ion suppression/enhancement experiments is described in Ref.…”

Liquid Chromatography for the Rapid Screening of Growth Promoters Residues in Meat

“…Applications to the analysis of veterinary drug residues have been recently reviewed (Niessen 1998;Balizs and Hewitt 2003;Gentili et al 2005). LC-tandem mass spectrometry has also been proposed as a simultaneous screening-confirmatory technique (Thevis et al 2003;Maurer et al 2004). The strategy may be based on multiple reaction monitoring of one precursor ion, transition product ion for each tested residue (i.e., steroids), using internal standards to allow for quantitation Hewitt et al (2002).…”

“…The coupling of mass spectrometry (MS)-MS can reduce the analysis time. The usual practice is the use of LC-MS with either atmospheric pressure chemical ionization (APCI; Maurer et al 2004;Puente 2004) or electrospray ionization (ESI; Thevis et al 2003;Hewitt et al 2002). Both ionization techniques produce negligible fragmentation.…”

Fluorometric Determination of Bopindolol and Celiprolol in Pharmaceutical Preparations and Biological Fluids

“…Several HPLC methods were published for the determination of CLP in pure form, pharmaceuticals, and biological fluids [23,24]. LC/MS was also utilized for the determination of CLP in combination with several drugs with the application to biological fluids [7,[25][26][27]. Different capillary electrophoretic methods were developed for the assay of CLP [28].…”