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Valese A.C.,Laboratorio Nacional Agropecuario SLAV Science LANAGRO RS | Valese A.C.,Federal University of Santa Catarina | Oliveira G.A.P.,Federal University of Santa Catarina | Kleemann C.R.,Laboratorio Nacional Agropecuario SLAV Science LANAGRO RS | And 2 more authors.
Journal of Food Composition and Analysis | Year: 2016

The development of rapid, high sample throughput methods is constantly demanded by food analytical laboratories. Several current methods for the analysis of ractopamine deal with time-consuming procedures or complicated sample pretreatment steps. Thus, this study aimed to validate and to optimize a simple method for the extraction of ractopamine from pork using a "Quick, Easy, Cheap, Effective, Rugged and Safe" (QuEChERS) approach. Extraction was carried out with an acetonitrile acidic solution and then sodium chloride was used to promote salting out, increasing the solubility of ractopamine. Anhydrous magnesium sulfate was added to remove water and the clean-up was carried out with C18 and primary/secondary amine. Ractopamine was then determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS) within 4.5min only, before a single extraction procedure. Full validation was performed in accordance to Commission Decision 2002/657/EC. Additionally, matrix effect, limit of detection (LoD), limit of quantitation (LoQ) and measurement uncertainty were also determined. Linear range was among 2.5-20μg/kg. LoD and LoQ were set to 1.5μg/kg and 2.5μg/kg, respectively, being below the maximum residue limit established by most countries. A high throughput screening and confirmatory tool, combined with a cheap and fast sample pretreatment method was developed. The method proved to be reproducible and sensitive and its applicability was checked on several samples of pork and pork products, with results that ranged from below LoQ to 6.54μg/kg. © 2016 Elsevier Inc. Source


Zarpelon J.,Laboratorio Nacional Agropecuario SLAV Science LANAGRO RS | Zarpelon J.,Federal University of Santa Catarina | Molognoni L.,Laboratorio Nacional Agropecuario SLAV Science LANAGRO RS | Valese A.C.,Laboratorio Nacional Agropecuario SLAV Science LANAGRO RS | And 3 more authors.
Journal of Food Composition and Analysis | Year: 2016

This work aimed to validate an automated method for acid hydrolysis and extraction of fat content of dulce de leche, a typical Latin American dairy product. Validation parameters were analyzed according to Commission Decision 657/2002/EC. The measurement uncertainty and the limits of detection (LoD) and quantification (LoQ) were also determined. Precision, recovery and decision limit were evaluated in two regulatory levels (6.0 and 9.0 g/100 g), with recoveries of 89% and 95%. The method was linear in the concentration range of 0.53-12.00 g/100 g and the LoD and the LoQ were set to 0.16 and 0.53 g/100 g, respectively. The validated method was compared to a Röse-Gottlieb reference method, presenting better precision in terms of repeatability and better recovery. Then, commercial samples, processed by inspected establishments in Argentina (n = 3), Uruguay (n = 2) and Brazil (n = 17) were analyzed and fat contents were among 1.10 and 10.12 g/100 g. Thus, this method is suitable for accurate routine analysis of the fat content of dulce de leche. © 2016 Elsevier Inc. Source

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