Specific features of amphenicol determination in foodstuffs by HPLC/high resolution quadrupole time-of-flight mass spectrometry

Resumo

simple method of sample preparation, identification, and determination of amphenicols in foodstuffs (chloramphenicol, chloramphenicol succinate, thiamphenicol, thiamphenicol glycinate acetylcysteinate, florfenicol, florfenicol amine) via high-performance liquid chromatography/high resolution quadrupole time-of-flight mass spectrometry by the exact masses of the ion that form in electrospray is proposed. The objects of analysis are meat (beef, pork, poultry), meat by-products, milk and dairy products, honey, and aquaculture products. Sample preparation consisted of extraction of the target components by acetonitrile and dilution of the extract twice with deionized water. Specific features in the determination of amphenicols and their derivatives associated with the emergence of various adducts in the electrospray device in the detection of both positive and negative ions were considered. A method of amphenicol determination by the addition method is proposed; it uses the summation of area signals of all registered adducts. The features and benefits of utilizing the method of standard additions are presented. The ranges of the defined contents are 0.1–10 ng/g for chloramphenicol and 1–100 ng/g for thiamphenicol and florfenicol. The relative standard deviation of the test results did not exceed 0.1; the duration of the analysis was 30–40 min.