Rapid method for the determination of tranquilizers and a beta-blocker in porcine and bovine kidney by liquid chromatography with tandem mass spectrometry

• Published in: Analytica chimica acta 2009-04, Vol.637 (1), p.185-192
• Main Authors: Mitrowska, Kamila, Posyniak, Andrzej, Zmudzki, Jan
• Format: Article
• Language: English
• Subjects: Acetonitrile; Acetonitriles - chemistry; Adrenergic beta-Antagonists - analysis; Adrenergic beta-Antagonists - isolation & purification; Analytical chemistry; Animals; Beta-blocker; Cattle; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Exact sciences and technology; Kidney; Kidney - chemistry; Kidneys; Liquid chromatography; Mass spectrometry; Mathematical analysis; Other chromatographic methods; Phenothiazines; Reproducibility of Results; Spectrometric and optical methods; Spectrometry, Mass, Electrospray Ionization - methods; Substance Abuse Detection - methods; Swine; Tandem Mass Spectrometry; Tranquilizers; Tranquilizing Agents - analysis; Tranquilizing Agents - isolation & purification
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2008.10.030

A fast and simple liquid chromatography with tandem mass spectrometry method for detection and confirmation of tranquilizers (chlorpromazine, propionylpromazine, acepromazine, triflupromazine, promazine, azaperone and its metabolite, azaperol) and beta-blocker (carazolol) in porcine and bovine kidney has been presented. The method relies on the extraction with acetonitrile followed by centrifugation. After evaporation of acetonitrile, the residue was reconstituted in a mobile phase and filtrated. The separation of analytes was performed on a C18 column using a mobile phase of acetonitrile and ammonium formate buffer (0.05 M, pH 4.5) with gradient elution. The electrospray ionization was used to obtain the protonated molecules [M+H] + and two product ions were monitored for each compound. For quantification deutered internal standards were used. The whole method has been validated according to the European Union requirements. Specificity, decision limit (CCα), detection capability (CCβ), trueness and precision were determined. The results showed good trueness ranged from 73.2% to 110.6% with a good R.S.D., less than 13.0% under within-laboratory reproducibility conditions. The calculated critical concentrations of CCα for phenothiazines were between 5.8 and 6.6 μg kg −1 while for azaperone CCα was 105.5 μg kg −1 and for azaperol was 121.4 μg kg −1. CCα for carazolol was 16.7 μg kg −1 in bovine and 21.9 μg kg −1 in porcine kidney. CCβ for phenothiazines were between 6.3 and 7.6 μg kg −1, for azaperone was 119.0 μg kg −1 and for azaperol was 140.0 μg kg −1. For carazolol in bovine kidney CCβ was 18.6 μg kg −1 whereas in porcine kidney was 24.4 μg kg −1.