Electrochemical methods for the determination of antibiotic residues in milk: A critical review.

Several antibiotics have been applied to veterinary medicine due to their broad-spectrum of antibacterial activity and prophylactic power. Residues of these antibiotics can be accumulated in dairy cattle, in addition to promoting contamination of the environment and, in more serious cases, in milk, causing a public health problem. Different regulatory agencies establish maximum residue limits for these antibiotics in milk, so it becomes important to develop sensitive analytical methods for monitoring these compounds. Electrochemical techniques are important analytical tools in analytical chemistry because they present low cost, simplicity, high sensitivity, and adequate analytical frequency (sample throughput) for routine analyses. In this sense, this review summarizes the state of the art of the main electrochemical sensors and biosensors, instrumental techniques, and sample preparation used for the development of analytical methods, published in the last five years, for the monitoring of different classes of antibiotics: aminoglycosides, amphenicols, beta-lactams, fluoroquinolones, sulfonamides, and tetracyclines, in milk samples. The different strategies to develop electrochemical sensors and biosensors are critically compared considering their analytical features. The mechanisms of electrochemical oxidation/reduction of the antibiotics are revised and discussed considering strategies to improve the selectivity of the method. In addition, current challenges and future prospects are discussed.

Simultaneous determination of cadmium, lead and copper in chocolate samples by square wave anodic stripping voltammetry.

In this work, an effective and simple method is proposed for the simultaneous determination of cadmium, lead and copper in chocolate samples by Square Wave Anodic Stripping Voltammetry (SWASV). An ultrasonic bath was used for the extraction of cadmium, lead and copper from fourteen chocolate samples using HNO3 solution (7 mol L-1). The electrochemical system consisted of a cell with three electrodes and HCl solution (10 mmol L-1) as the supporting electrolyte. An efficient extraction of the metals (~100%) was attained after 1 h of ultrasonic pre-treatment. Quantitative analysis was carried out by the standard addition method. Good linearity, precision and accuracy were obtained in the range of concentrations examined. The accuracy was evaluated by means of a reference sample of spiked skim milk powder (BCR 151) to prove the reliability of the method. Detection limits (LOD) of 0.089, 0.059 and 0.018 µg g-1 were found for cadmium, copper and lead, respectively, in the chocolate samples. Concentrations in chocolate samples were 4.30-138 µg g-1 for Cu and 0.83-27.9 µg g-1 for Pb, with no significant Cd. The simultaneous determination brings advantages to other methods already reported for chocolate analysis and the samples preparation proposed avoids the traditional sample mineralization step. These characteristics show this new method is especially attractive for case studies and routine analysis.

Multivariate approach to assess in vitro Fe bioaccessibility in chicken meat

Abstract A 32 factorial design was employed to develop an in vitro digestion method for estimation of Fe bioaccessible fractions in cooked chicken meat. The effects of sample size and the in vitro bioaccessible fractions of this essential element were evaluated. A sample preparation method employing a microwave assisted digestion with dilute nitric acid was used prior to total Fe determination. For the bioacessibility studies, the optimized procedure employed 7.5 g of sample and 6% w/v of an acid pepsin solution. This procedure was applied to two kinds of chicken meat samples: breast and liver. Flame Atomic Absorption Spectrometry was used to determine total and bioaccessible (chyme or soluble portion) levels of iron in the samples. With respect to total Fe content, the bioaccessible fractions of Fe found in these samples were around 23% and 56 %, for breast and chicken liver, respectively. The chicken liver sample showed the highest total (400 ± 10 mg kg-1) and bioaccessible Fe contents (223 ± 18 mg kg-1) and stands out as a good source of this micronutrient.

Classification of frankfurters by FT-Raman spectroscopy and chemometric methods.

Frankfurters are widely consumed all over the world, and the production requires a wide range of meat and non-meat ingredients. Due to these characteristics, frankfurters are products that can be easily adulterated with lower value meats, and the presence of undeclared species. Adulterations are often still difficult to detect, due the fact that the adulterant components are usually very similar to the authentic product. In this work, FT-Raman spectroscopy was employed as a rapid technique for assessing the quality of frankfurters. Based on information provided by the Raman spectra, a multivariate classification model was developed to identify the frankfurter type. The aim was to study three types of frankfurters (chicken, turkey and mixed meat) according to their Raman spectra, based on the fatty vibrational bands. Classification model was built using partial least square discriminant analysis (PLS-DA) and the performance model was evaluated in terms of sensitivity, specificity, accuracy, efficiency and Matthews's correlation coefficient. The PLS-DA models give sensitivity and specificity values on the test set in the ranges of 88%-100%, showing good performance of the classification models. The work shows the Raman spectroscopy with chemometric tools can be used as an analytical tool in quality control of frankfurters.