Determination of 8α-hydroxymutilin as a Marker Residue for Tiamulin in Swine Tissue by Liquid Chromatography-Tandem Mass Spectrometry
| Autor: | Hiroshi Akiyama, Shizuka Saito-Shida, Satoru Nemoto, Nao Kashiwabara |
|---|---|
| Rok vydání: | 2021 |
| Předmět: |
Detection limit
Residue (complex analysis) Chromatography 010401 analytical chemistry Tiamulin 04 agricultural and veterinary sciences 040401 food science 01 natural sciences Applied Microbiology and Biotechnology 0104 chemical sciences Analytical Chemistry Matrix (chemical analysis) chemistry.chemical_compound 0404 agricultural biotechnology chemistry Liquid chromatography–mass spectrometry media_common.cataloged_instance Veterinary drug European union Safety Risk Reliability and Quality Safety Research Pleuromutilin Food Science media_common |
| Zdroj: | Food Analytical Methods. 14:845-855 |
| ISSN: | 1936-976X 1936-9751 |
| DOI: | 10.1007/s12161-020-01950-w |
| Popis: | Tiamulin is a semi-synthetic derivative of the natural antibiotic pleuromutilin and is widely used as a veterinary drug for swine. Herein, we report the development of a sensitive and reliable method for determining 8α-hydroxymutilin as a marker residue for tiamulin in swine tissue using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method consists of sample extraction with acetone, defatting by acetonitrile/hexane partitioning, hydrolysis of the tiamulin metabolites to 8α-hydroxymutilin under alkaline conditions, liquid-liquid extraction with ethyl acetate, cleanup using a primary secondary amine cartridge, and LC-MS/MS analysis. The developed method was validated for 8α-hydroxymutilin in swine muscle, fat, and liver at two levels, namely 0.01 mg/kg and the maximum residue limits established in Japan (i.e., 0.1 mg/kg for swine muscle and fat, and 0.6 mg/kg for liver). The trueness ranged from 82 to 89%, and the relative standard deviations ranged from 1 to 3%. No chromatographic interference was observed near the retention time of 8α-hydroxymutilin, and matrix effects were negligible for all matrices, suggesting that the cleanup protocol was effective. The calibration curve was linear in the 0.005–0.5 μg/mL range, with a coefficient of determination greater than 0.997. The developed method enabled accurate quantification using solvent-based calibration without compensating for matrix effects and losses during sample preparation. The limit of detection of the method was 0.0005 mg/kg for each matrix. The developed method is suitable for regulatory-purpose analysis of 8α-hydroxymutilin as a marker residue for tiamulin as defined by the European Union and several other countries. |
| Databáze: | OpenAIRE |
| Externí odkaz: |
|
Full text from SpringerLink