Two analytical methods for determination of five antibiotics classes in surface water and drinking water samples were developed and validated based on solid phase extraction followed by high-performance liquid chromatography coupled to tandem mass spectrometry. Two distinct chromatographic gradients were used according to the polarity of the different pharmaceuticals. The methods were applied for the quantification of 46 analytes belonging to beta-lactams, macrolides, fluoroquinolones, sulfonamides and tetracyclines classes. Validation results showed recoveries above 75% for the studied analytes in water samples. The method limits of detection calculated for the surface water and drinking water samples were, respectively, from 1 to 12 ng L -1 and from 0.15 to 20 ng L -1 . The method limit of quantification ranged from approximately 3 to 38 ng L -1 for surface water samples and from 0.5 to 64 ng L -1 for drinking water samples. The methods showed to be linear over the range of 25 to 1000 ng L -1 with coefficients of determination greater than 0.94. Amoxicillin, cephalexin and sulfamethoxazole as high as 105 ng L -1 were found in surface water and erythromycin, azithromycin and clarithromycin up to 35 ng L -1 could also be found in surface water. Clarithromycin, cefaclor, oxacillin, sulfamethoxazole and troleandomycin were detected in the lower range up to 10 ng L -1 in drinking water.
EVALUATION OF DIFFERENT EXTRACTION METHODS FOR IDENTIFICATION OF MACROLIDES RESIDUES IN MEAT-BASED CANNED BABY FOOD BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY (LC-MS/MS). The interest in a better quality of life raised the concern about food safety. The administration of veterinary drugs in livestock may lead the occurrence of residues in food that may be harmful to consumers. Processed products are being consumed more and more, which increases concern for the safety of infants and children because they are more susceptible physiologically. Among these products stand out canned baby foods, defined by Ordinance 34/1998 issued by Brazilian Ministry of Health. Eggs and meat-based salty products for infants and children, legally designated as soups, fit into this definition and can not contain residues of hormones, antibiotics, as well as other pharmacologically active substances. Several techniques are used as identification and confirmatory assays of veterinary drug residues in food, although the main used technique is liquid chromatography-tandem mass spectrometry (LC-MS/MS). The aim of this work was to make a comparative assessment between different extraction methods in order to establish the best condition within the tested ones for the identification of macrolide residues in meat-based canned baby food by LC-MS/MS. A simple and effective extraction method, with good recoveries (65-93%) and satisfactory relative standard deviations (0.4-11%), was achieved using QuEChERS procedure for sample preparation.
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