A rapid method to determine antibiotic residues in milk using liquid chromatography coupled to electrospray tandem mass spectrometry

Abstract

Atualmente, existe uma preocupação mundial sobre qualidade de vida e um dos requisitos mais importantes é ingerir alimentos seguros e nutritivos. A administração de antibióticos em gado para tratamento de diversas doenças infecciosas tem contribuído para a contaminação do leite industrializado. Por isso, o principal objetivo deste trabalho foi desenvolver um método simples e rápido para identificar e quantificar quatorze antibióticos de diferentes classes em leite, dentre estes: cinco β-lactâmicos, quatro sulfonamidas, três tetraciclinas, um macrolídeo e uma cefalosporina, utilizando sistema de CLAE em modo reverso de eluição com ionização por electrospray e detecção por espectrometria de massas do tipo triploquadrupolo (MS/MS). Esta técnica utilizada em modo de aquisição Monitoramento Múltiplo de Reação (Multiple Reaction Monitoring -MRM) permitiu a determinação dos compostos propostos na faixa de concentração de 0,75 a 375 µg L -1 , com coeficientes de linearidade (r) maiores do que 0,9960, seletividade, sensibilidade e velocidade, com tempo total de análise menor do que 10 minutos. Os compostos dicloxacilina e eritromicina apresentaram o maior e menor resultado de limite de decisão (ccα) igual a 0,05 e 9,77 µg L -1 , respectivamente. Em geral, os resultados de recuperação foram de 65 a 125%, com valores de desvio padrão de 2,0 a 15%. Este método também foi aplicado para avaliar a qualidade de diferentes marcas de leite integral disponíveis no mercado brasileiro.There is a common worldwide concern about the quality of life and one of the most important requirements is to ingest safe and nutritious food. The administration of antibiotics in cattle to treat several infectious diseases has contributed to the contamination of industrialized milk. The goal of this work was to develop a simple and fast method to identify and quantify fourteen antibiotics from different classes in milk, including five β-lactams, four sulfonamides, three tetracyclines, one macrolide and one cephalosporin, using reversed-phase liquid chromatography with electrospray ionization and triple quadrupole mass spectrometry (MS/MS). This technique used Multiple Reaction Monitoring (MRM) acquisition mode to allow the determination of the proposed compounds in the concentration range from 0.75 to 375 µg L -1 , within coefficient of linearity (r) higher than 0.9960, selectivity, sensitivity, and speed, with analysis time less than 10 minutes. Dicloxacillin and erythromycin showed the lower and higher decision limits (ccα) results of 0.05 and 9.77 µg L -1 , respectively. Overall, the recoveries results ranged from 65 to 125%, with standard deviation values from 2.0 to 15%. This method was also applied to evaluate the quality of different fat milk brands offered in the Brazilian market.

Determination of L-Ascorbic Acid in Milk by Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry Analysis

“…6,12,15 Organic solvents, such as ethanol, acetone and acetonitrile, have also been reported as protein precipitating agents in milk and other samples. 14,[16][17][18][19] Several analytical methods have been reported for the determination of vitamin C, e.g., enzymatic, 20 spectrophotometric 21 and separation techniques such as high-performance liquid chromatography (HPLC), which provide more accurate results. HPLC has been used extensively for L-AA determination in various foods, 7,8,[22][23][24][25] including milk.…”

Development of a multi-class method for the identification and quantification of residues of antibiotics, coccidiostats and corticosteroids in milk by liquid chromatography–tandem mass spectrometry

“…in the study, i.e., diclazuril. Positive ionization was already reported for the selected drugs (Martins-Júnior, Kussumi, Wang, & Lebre, 2007;Olejnik et al, 2009). The next step was to select an adequate analytical column.…”

Surface Plasmon Resonance Nanosensors for Detecting Amoxicillin in Milk Samples with Amoxicillin Imprinted Poly(hydroxyethyl methacrylate‐N‐methacryloyl‐(L)‐ glutamic acid)

“…Antibiotics are antimicrobial drugs used to kill or prevent the growth of bacterias . Amoxicillin (AMOX) is a semi‐synthetic antibiotic used to treat many bacterial infections.…”