Determination of lincomycin and tylosin residues in honey using solid-phase extraction and liquid chromatography-atmospheric pressure chemical ionization mass spectrometry

Aspectos analíticos e regulatórios na determinação de resíduos de macrolídeos em alimentos de origem animal por cromatografia líquida associada à espectrometria de massas

“…17 Ácidos carboxílicos perfluorados podem ser eventualmente utilizados como pares iônicos hidrofóbicos para melhorar a forma dos picos cromatográficos. 24,45 No entanto, sabe-se que pares iônicos podem causar supressão iônica no caso da ionização por eletronebulização (Electrospray Ionization -ESI), devido à pareação iônica durante o processo de ionização na fonte, provocando perdas significativas no sinal analítico, especialmente em compostos que possuem nitrogênio em suas moléculas. Portanto, pares iônicos devem ser evitados sempre que possível na análise de traços de macrolídeos.…”

Trace analysis of antibacterial tylosin A, B, C and D in honey by liquid chromatography-electrospray ionization-mass spectrometry

“…To solve this problem, different mobile phases, suggested in the bibliography for the analysis of TA and other macrolides, were tested. There are mainly ternary mobile phases consisting of mixtures of ACN-formic acid-water [10]; methanol-01% v/v TFA in ACN or 0.1% v/v TFA in water [22]; methanol-ACN-oxalic acid [24]; ACN-heptafluorobutiric acid-ethyl acetate [23]; water-potassium phosphate buffer-THF [26]. Also, some binary mobile phases have been proposed [21,27].…”

“…Microbiological assays were firstly used, but due to their lack of specificity chromatographic techniques were preferred. LC with UV detection at 280 nm [11] was used, although the coupling LC-MS results were more suitable, because this technique allows better identification, providing good detection limits for TA and other potentially present antibiotics [10,21,23]. With regard to the sample preparation, the most common procedures include a dilution of sample at alkaline pH and an isolation step based on the use of SPE on C18 or polymeric cartridges [10,[21][22][23].…”

Study on the interaction between palladium(II)–lincomycin chelate and erythosine by absorption, fluorescence and resonance Rayleigh scattering spectra and its analytical applications

“…As a well-established drug used in human and veterinary medicine, it is mainly active against Gram-positive bacteria and has been applied in the treatment of various illnesses, including mouth and upper respiratory tract infections and skin infections (2,3). Various methods have been described in the literature for the analysis of Linco, such as microbiological assay (4), thin layer chromatography (TLC) (5), gas chromatography (6), highperformance liquid chromatography (HPLC) (7)(8)(9)(10)(11), liquid chromatography-mass spectrometry (LC-MS) (12)(13)(14)(15), electrochemistry (16)(17)(18), capillary electrophoresis (CE) (19,20), atomic absorption spectrometry (21) and spectrophotometry (SP) (21)(22)(23)(24)(25). However, these methods all have their advantages and disadvantages: microbiological assays were originally used, but they need long-term culture and are non-specific; TLC methods have strong separation capability and only need small amount of sample, but suffer from poor reproducibility; CE and SP methods are not sensitive enough for the determination of trace Linco; HPLC methods are efficient and fast but, because Linco lacks sufficient UV absorption, a pre-or post-column derivation procedure is normally required to improve sensitivity; LC-MS methods are very sensitive but the expensive equipment can not be afforded by every laboratory.…”