A confirmatory multi-residue method has been developed to allow for the detection, confirmation and quantification of eleven coccidiostats in animal feed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method can be used to determine halofuginone, robenidine, nicarbazin, diclazuril, decoquinate, semduramicin, lasalocid, monensin, salinomycin, narasin, maduramicin at levels relating to unavoidable carry over as stated in Regulation 2009/8/EC. Feed samples are extracted with water and acetonitrile with the addition of anhydrous magnesium sulphate and sodium chloride.
View Article and Find Full Text PDFA confirmatory method has been developed to allow for the analysis of fourteen prohibited medicinal additives in pig and poultry compound feed. These compounds are prohibited for use as feed additives although some are still authorised for use in medicated feed. Feed samples are extracted by acetonitrile with addition of sodium sulfate.
View Article and Find Full Text PDFRapid 'on-site' methods are required by the pork industry to screen for the presence of antibiotic residues in meat and meat products. There are few rapid and easy-to-use methods suitable for application in non-analytical laboratories. This paper describes a novel approach for the screening of sulfamethazine in pork muscle using matrix solid phase dispersion, a microcolumn preconcentration step and thin-layer chromatographic detection.
View Article and Find Full Text PDFA new extraction method for the acetylgestagens medroxyprogesterone acetate (MPA), chloromadinone acetate and megestrol acetate, from kidney fat, has been developed. The method is a combination of matrix solid phase dispersion and solid phase extraction and is simpler and safer than previous methods, especially as it can be automated. The recovery was estimated as 59 +/- 5% (mean +/- standard deviation) for MPA.
View Article and Find Full Text PDFA modified high-performance liquid chromatographic method has been developed for the determination of ivermectin (IVM) residues in fish muscle tissue. The extraction and clean-up procedure is based on the matrix solid phase dispersion technique. Control and IVM-fortified fish muscle samples (0.
View Article and Find Full Text PDFA rapid and simple extraction/clean-up procedure (matrix solid phase dispersion, MSPD) for the determination of sulphamethazine (SMZ) in pork muscle tissue is compared with a solvent extraction method. Extracts of samples fortified with SMZ or of incurred samples were found to be free from interfering compounds when chromatographed using HPLC or TLC separation systems. Recovery of SMZ from fortified samples is greater than 80% and residue levels of incurred samples found using the MSPD procedure compare favourably with results obtained using the solvent extraction method.
View Article and Find Full Text PDFA sensitive and selective high-performance liquid chromatographic procedure is described for the determination of the synthetic corticosteroid dexamethasone (DXM), in bovine muscle, kidney, liver and fat tissues, using methylprednisolone as the internal standard. Following extraction with ethyl acetate (muscle, kidney and liver) or diethyl ether (fat) and clean-up of the tissue extract, the drug residue was isolated using a C18 solid-phase extraction column. Separation of DXM was achieved by reversed-phase high-performance liquid chromatography with ultraviolet detection at 254 nm.
View Article and Find Full Text PDFAn alumina stationary phase has been assessed in the study of the retention behaviour of the anticancer drug cisplatin and its major hydrolysis products. Parameters such as buffer concentration in the mobile phase, pH, organic modifier and competing ion have been investigated in order to optimize chromatographic separation with ultraviolet detection. The separation scheme developed has been used to monitor the hydrolysis of cisplatin in aqueous and saline media, and to monitor the interaction of hydrolysed solutions of cisplatin with the amino acid cysteine.
View Article and Find Full Text PDFThe interaction of the anti-cancer drug cisplatin with human serum albumin and cystine has been investigated using differential pulse adsorptive voltammetry. Based on an understanding of the voltammetric behaviour of these biological molecules, which rely on the presence of the disulphide groups within their molecular structure for their electroactivity, it has been postulated that binding of cisplatin to these molecules occurs at the disulphide bond. A fractional coefficient for the binding of cisplatin to human serum albumin at pH 7.
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