Improving the selectivity and sensitivity for quantifying 8-α-hydroxy-mutilin in rabbit tissues by using basic mobile phases and negative ionization
| Autor: | Gordon T. Bolger, Guifen Gu, Yanxin Wu, Aimin Tan, John C. Fanaras, Xuan Gui, Albert Licollari |
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| Rok vydání: | 2017 |
| Předmět: |
Electrospray
Meat Clinical Biochemistry Analytical chemistry Tiamulin Mass spectrometry 01 natural sciences Biochemistry Analytical Chemistry chemistry.chemical_compound Drug Stability Liquid chromatography–mass spectrometry Limit of Detection Tandem Mass Spectrometry Animals Polycyclic Compounds Residue (complex analysis) Chromatography 010405 organic chemistry Chemistry Muscles 010401 analytical chemistry Polyatomic ion Pesticide Residues Reproducibility of Results Cell Biology General Medicine Ketones 0104 chemical sciences Liver Nonlinear Dynamics Rabbits Diterpenes Selectivity Pleuromutilin Chromatography Liquid |
| Zdroj: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. 1072 |
| ISSN: | 1873-376X |
| Popis: | Previously reported LC–MS methods for quantifying 8-α-hydroxy-mutilin (a marker residue of tiamulin) in tissues all used a pseudo MRM transition (from protonated molecular ion to protonated molecular ion, m/z 337 → 337) due to difficulties in finding a product ion, leading to suboptimal selectivity and sensitivity for detection. By using electrospray negative ionization in a basic medium, we, for the first time, found a highly selective and sensitive true MRM transition for 8-α-hydroxy-mutilin, m/z 335 → 179. With this newly found MRM transition and the use of pleuromutilin as the internal standard, a very sensitive, selective, and robust LC–MS/MS method has been developed and validated for quantifying 8-α-hydroxy-mutilin in rabbit tissues (muscle, liver, kidney, and fat). In comparison with the previously published methods, the selectivity and sensitivity were significantly improved. For the concentration range validated (0.2–10 ppm or 0.2–10 μg/g), the within-run and between-run accuracies (% bias) ranged from −5.0 to 3.1 and −4.9 to 3.0, respectively. The% CV ranged from 2.2 to 6.6 and 4.7 to 8.3 for within-run and between-run precisions, respectively. The validated method was successfully used to support two GLP tissue residue depletion studies in rabbits. |
| Databáze: | OpenAIRE |
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