Effect of high hydrostatic pressure on the oxidation of washed muscle with added chicken hemoglobin.

The role of chicken hemoglobin in lipid oxidation of washed chicken muscle exposed to high hydrostatic pressure (0, 200, 400 and 600 MPa) was examined. The observed decrease in redness was higher with elevated pressures (5.0 vs 3.7). During storage, redness decreased in samples exposed to 400 and 600 MPa. This decrease was concomitant with the progression of oxidation and the 2.5 fold decrease of soluble heme. An additional experiment was conducted to examine the effect of the hemoglobin mode of addition into pressurized muscle. The exposure at 600 MPa led to washed muscle oxidation even in the absence of hemoglobin, thus indicating that pressure treatments triggered lipid oxidation. However, the presence of native or pressurized hemoglobin into pressurized washed muscle caused more hexanal than the pressurized control without hemoglobin. Overall, results suggest that membrane disruption and the release of hemin are crucial for the onset of oxidation.

Immunochemical determination of fluoroquinolone antibiotics in cattle hair: a strategy to ensure food safety.

Enrofloxacin (ERFX) is a synthetic antibiotic of the fluoroquinolone (FQ) family, which is commonly administered in veterinary medicine. ERFX and its metabolite, ciprofloxacin (CPFX), have been reported to accumulate in hair of treated animals. Therefore, hair analysis is an attractive non-invasive alternative to control misuse of such antibiotic and to ensure food safety by preventing such food derived products arrive to the consumer. In this context, an immunochemical analytical protocol has been established to detect ERFX and CPFX residues in cattle hair samples. Unpigmented and pigmented hair were collected from ERFX-treated and non-treated calves, and the aqueous NH4OH extracts were directly analyzed by ELISA, being possible to achieve limits of detection in the range of 10-30 µg kg(-1). A good concordance between HPLC and ELISA measurements was observed. The results demonstrate the potential of the immunochemical procedure reported here to rapidly screen and quantitate FQ residues in hair samples.

Analysis of eleven phenolic compounds including novel p-coumaroyl derivatives in lettuce (Lactuca sativa L.) by ultra-high-performance liquid chromatography with photodiode array and mass spectrometry detection.

INTRODUCTION: Lettuce is a widely consumed vegetable and a good source of phenolic compounds. Several factors (genetic, agronomical and environmental) can influence the lettuce composition; their effects are not completely defined and more studies are needed on this topic. OBJECTIVE: To develop an improved ultra-high-performance liquid chromatography (UHPLC) method to quantify the main target intact phenolic compounds in lettuce. METHODOLOGY: UHPLC identification of the compounds was supported by PAD spectra and MS(n) analyses. Quantification was carried out by PAD, by creating matrix-matched calibration curves at the specific wavelength for each compound. RESULTS: Sample pretreatment was simplified, with neither purification nor hydrolysis steps. Chromatographic conditions were chosen to minimise matrix interferences and to give a suitable separation of the major phenolic compounds within 27 min. The method allowed the quantification of 11 intact phenolic compounds in Romaine lettuces, including phenolic acids (caffeoyl and p-coumaroyl esters) and flavonoids (quercetin glycosides). Four p-coumaroyl esters were tentatively identified and quantified for the first time in lettuce. CONCLUSION: The main intact phenolic compounds, including four novel p-coumaroyl esters, were simultaneously quantified in lettuce with optimal performances and a reduced total time of analysis. These findings make headway in the understanding of the lettuce phytochemicals with potential nutritional relevance.

Traceability of sulfonamide antibiotic treatment by immunochemical analysis of farm animal hair samples.

The use of hair to trace use of unauthorized substances, therapeutic agents, or their misuse is becoming very attractive since residues can be detected for a long time after treatment. For this purpose, an indirect enzyme-linked immunosorbent assay (ELISA) has been evaluated for its capability to trace sulfonamide antibiotic treatment by analyzing cattle and pig hair samples. Pigmented and nonpigmented hair samples from control and sulfamethazine (SMZ)-treated pigs and calves were collected, extracted under different alkaline conditions, and analyzed by ELISA after just diluting the extracts with the assay buffer. Data analysis following the European recommendations for screening methods demonstrates that the ELISA can detect SMZ in hair samples with a limit of detection (90% of the zero dose (IC(90))) between 30 and 75 ng g(-1). The same samples have been analyzed by HPLC after a dual solid-phase extraction. The ELISA results matched very well those obtained by the chromatographic method, demonstrating that the immunochemical method can be used as a screening tool to trace animal treatments. Between the benefits of this method are the possibility to directly analyze hair extracts with sufficient detectability and its high-throughput capability. Preliminary validation data are reported using an experimental approach inspired on the Commission Decision 2002/657/EC criteria for screening methods.

Formation of tetracycline degradation products in chicken and pig meat under different thermal processing conditions.

Tetracycline (TC) and 4-epitetracycline (4eTC) degradation, as well as anhydrotetracycline (ATC) and 4-epianhydrotetracycline (4eATC) formation, has been evaluated in thermally treated chicken breast, pig loin, and pig loin with added back-fat. Samples containing TC and 4eTC residues were submitted to microwave or boiling heating, extracted with a mixture of McIlvaine buffer/methanol (75:25), and analyzed by high-performance liquid chromatography-diode array detection on a phenyl-hexyl reverse phase chromatographic column. The formation of ATC and 4eATC, as well as of two unidentified compounds, was described for the first time in edible meat samples submitted to mild thermal treatments, similar to those applied at home to cook foods. Degradation of TC and 4eTC and formation of ATC and 4eATC versus time of treatment fitted satisfactorily a first-order kinetic. Even if the potential toxic effects of these breakdown compounds should be further investigated, their formation in cooked meat should be taken into account when maximum residue limits are established.

Assessment of enrofloxacin and ciprofloxacin accumulation in pig and calf hair by HPLC and fluorimetric detection.

Enrofloxacin is a synthetic bacteriostatic administered in veterinary therapy. It can also be used illegally as a growth promoter to enhance feed efficiency and weight gain. This practice is banned in several countries due to its potential negative effects on the environment and human health. A suitable method for extracting and quantifying enrofloxacin (ENR) and its main metabolite ciprofloxacin (CPR) in cattle and pig hair by high-performance liquid chromatography-fluorimetric detection (HPLC-FLD) had been proposed. ENR and CPR were extracted from hair samples with methanol acidified with trifluoroacetic acid for 24 h at 70 degrees C. The extracts were evaporated and redissolved in the mobile phase before injection. This simplified procedure enabled the detection of both CPR and ENR at ng g-1 levels (limit of detection 4-5 ng g-1) without further purification. Detectable residues of ENR were found in calf and pig hairs after the pharmacological treatment was started. Mean concentrations of quinolone (ENR, CPR) in contaminated hairs ranged from 20 to 2,518 ng g-1 in calves and from 152 to 1,140 ng g-1 in pigs. Hair pigmentation enhanced quinolone accumulation significantly. Hair analysis seems to increase the time window available for the retrospective detection of illegal ENR administration compared to edible tissue analysis.

Influence of volatile compounds on the development of off-flavours in pig back fat samples classified with boar taint by a test panel.

Dynamic Head Space methodology was applied to evaluate the possible contribution of some volatile compounds to the development of boar taint in pig backfat samples with low concentrations of skatole and androstenone, but which had previously been classified as tainted by a trained test panel. Volatile compounds were collected in a trap of graphited charcoal and analysed by GC-MS in Scan mode. Aldehydes and short chain fatty acids, compounds that play a significant role in the development of undesirable aromas in food products, were the main classes of compounds identified in this study, although the possible contribution of other compounds that were detected in a minor proportion - such as alcohols and ketones - was evaluated. Styrene and 1,4-dichlorobenzene, compounds that may have come from an external contamination, showed a high concentration in the samples classified with boar taint, so these compounds could have been responsible for the development of some off-flavours in the fat samples studied in this work. In the same study, skatole and androstenone were also determined by normal phase HPLC and GCMS, respectively.

Residue analysis of macrolides in poultry muscle by liquid chromatography-electrospray mass spectrometry.

A liquid chromatography-mass spectrometry method is proposed for the determination of seven macrolides authorised in the EU as veterinary drugs for food-producing animals. Sample treatment involves extraction of the analytes with a water-methanol mixture containing metaphosphoric acid and clean-up by SPE with a cation-exchange cartridge. Separation was carried out in an end-capped silica-based C18 column and mobile phases consisting of water/acetonitrile mixtures containing trifluoroacetic acid. A gradient elution, from 28 to 40% acetonitrile was used. Detection was performed by mass spectrometry with electrospray ionisation in the positive mode. Several parameters affecting the mass spectra were studied. The protonated molecular ion was selected for quantitation purposes under selected ion monitoring mode. Detection limits were in the range 1-20 microg l(-1). Recoveries ranged between 56 and 93% with RSD lower than 12%. The method has been successfully applied for multiresidue determination of seven macrolides below the MRLs established by the European Union.

Influence of meat quality and NaCl percentage on glutathione peroxidase activity and values for acid-reactive substances of raw and dry-cured Longissimus dorsi.

Fresh and dry-cured porcine loins (Longissimus dorsi) were analysed for glutathione peroxidase (GSHPx) activity and acid reactive substances (TBARS) in order to assess the influence of meat quality and salt (NaCl) concentration on oxidative stability. The results showed lower GSHPx activity and higher TBA levels in normal meat than in PSE meat indicating a higher oxidative stress in normal meat quality. GSHPx remained active at the end of the curing process. Higher salt concentration led to lower enzyme activity and TBARS values prompted the thought of a double role of NaCl as an enzyme inhibitor and as an antioxidant molecule.