The Development And Validation Of A Rapid Method For The Determination Of Antibiotics In Milk By High-pressure Liquid Chromatography-tandem Mass Spectrometry
Abstract
O. V. Bayer, O. S. Yaremchuk, L. V. Shevchenko, V. M. Mykhalska
On the basis of the conducted research, validation of the method for the determination of sulfonamides and antibiotics in milk by screening method was developed and conducted by LC / MS / MS. It has been confirmed that a method determination by ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC / MS / MS) is more sensitive and selective. Validation of the method was carried out in accordance with the Decision of the European Commission 2002/657 / EC of 12 August 2002, which ensures the implementation of Council Directive 96/23 / EC concerning the effectiveness of analytical methods and the interpretation of results, and in accordance with the recommendations of the reference laboratories of the European Union CRLs of 20/1/2010 on the assessment of the suitability of screening methods for the determination of veterinary drugs. It is proved that the adapted method for the determination of sulfonamides and antibiotics is sensitive and according to parameters meets the European requirements. This method is fast enough, practical and universal, since it allows simultaneous examination of about 70 antibacterial drugs at the same time in milk. It has been established that the method of determining the residual amount of sulfonamides and antibiotics by the UPLC / MS / MS is suitable for the investigation of milk on the content of the following drugs: sulfaguanidine, sulfacetamide, sulfapiridine, sulfadiazine, sulfamethoxazole, sulfathiazole, sulfamethazine, sulfamethizole, sulfabenzamide, sulfaquinoxaline, sulfadoxine, sulfadimetoxin, sulfanilamide, trimethoprim, sulfamonomethoxine, sulfamethoxypyridazine, sulfachlorpyridazine, sulfamoxol, dapsone, amoxicillin, ampicillin, penicillin G, penicillin V, oxacillin, cloxacillin, nafcillin, dicloxacillin, cefalonium, cefazolin, cefoperazon, cefquinome, cefapirin, ceftiofur, cefalexin, norfloxacin, enrofloxacin, ciprofloxacin, marbofloxacin, difloxacin, danofloxacin, sarafloxacin, flumekvin, oxolinic acid, nalidixic acid, oxytetracycline, chlortetracycline, tetracycline, doxycycline, epi-oxytetracycline, epi-tetracycline, epi-chlortetracycline, streptomycin, dihydrostreptomycin, gentamicin, kanamycin, apramycin, paromomycin, lincomycin, spectinomycin, tilmycosin, erythromycin, josamycin, spiramycin, tylosin, tiamulin, colistin, gamitromycin, tulatromycin. In assessing the suitability of the method, the MS / MS detection parameters are set and the validation characteristics are determined.
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