Food Analysis

This work reports a method for extraction and analysis of thiosultap sodium, thiocyclam, and nereistoxin in pepper. Different extraction methods were tested to attain the best recoveries. The final extraction method combines acetonitrile extraction in an acidic medium with ultrasonic extraction followed by a cleanup step with anhydrous MgSO(4). The analyses were performed on a Linear Ion Trap Quadrupole LC-MS/MS in negative mode for thiosultap sodium and in positive mode for thiocyclam and nereistoxin. Recovery studies carried out on peppers spiked at different fortification levels (20 and 200 μg∙kg(-1)) yielded average recoveries in the range 58-87% with RSD (%) values below 20%. Calibration curves covering two orders of magnitude were performed and they were linear over the concentration range studied (0.001-0.5 mg∙l(-1)). Instrumental detection limits were in the low μg∙kg(-1) range. Stability studies of thiosultap sodium in water were performed by evaluating a 100-μg∙l(-1) solution of this compound in water. It was analyzed over 7 days, after which more than 80% degradation of thiosultap sodium could be observed.

A sensitive, precise and accurate method has been developed for the simultaneous determination of T-2 and HT-2 toxins in cereal grains at ppb levels using high-performance liquid chromatography (HPLC) with fluorescence detection and 1-antroylnitrile (1-AN) as labeling reagent after immunoaffinity clean-up. Cereal samples were extracted with methanol/water (90:10, v/v), and the extracts were cleaned-up through commercially available immunoaffinity columns containing

Rapid advances in biosensors have recently been reported. This has been possible due to rapid growth in the development of new biomaterials such as conducting polymers, copolymers and sol gels etc and the reported improvements in sensing techniques. Biosensors are miniaturized devices employing biochemical molecular recognition as the basis for a selective analysis. The response generated as a result of biochemical reaction is detected by a transducer to give a signal (optical/electrical/thermal) that can be used with or without amplification for the estimation of the concentration of an analyte in a given test sample. Among the various biosensors, electrochemical sensors, especially amperometric biosensors presently hold a leading position.Due to specificity, portability, simplicity, high sensitivity, potential ability for real-time and on-site analysis coupled with the speed and low cost, biosensors have been projected to have applications in food analysis, environment control, clinical detection, drug and agriculture industries etc. Besides this, biosensors offer exciting opportunities for numerous decentralized clinical applications, ranging from emergency room screening, home self testing and alternative site testing, continuous and real-time in vivo monitoring. New generation of biosensors combining new bioreceptors with the ever-growing number of transducers is emerging. The present paper highlights some of the recent advances in the area of biosensors contributed by our laboratory.

A method was validated for the multi-residue analysis of 82 pesticides in grapes at ≤25 ng/g level. Berry samples (10 g) mixed with sodium sulphate (10 g) were extracted with ethyl acetate (10 mL); cleaned by dispersive solid phase extraction and the results were obtained by liquid chromatography–tandem mass spectrometry. Reduction in sample size and proportion of ethyl acetate for extraction did not affect accuracy or precision of analysis when compared to the reported methods and was also statistically similar to the QuEChERS technique. The method was rugged (HorRat < 0.5) with <20% measurement uncertainties. Limit of quantification was <10 ng/g with recoveries 70–120% for most pesticides. The method offers cheaper and safer alternative to typical multi-residue analysis methods for grape.

Populations in North India depend on a number of vegetable crops of which Amaranthus spp. is the most important since it is the only crop available in the hot summer months when no other foliage crop grows in the field. However, reports on mineral composition of leaves are rare with absolutely no information on the qualitative improvement of foliage yield with special reference to minerals. Studies on correlation among the minerals as well as with yield and leaf attributes are also lacking. Hence, we report the proximate mineral composition in 30 strains of A. tricolor along with some suggestions for qualitative improvement of the foliage yield with reference to minerals. Our study showed that vegetable amaranth is a rich source of minerals like calcium (1.7±0.04 g/100 g), iron (1233.8±50.02 mg/kg), and zinc (791.7±28.98 mg/kg). The heritability estimates were high for most of the traits, with potassium and calcium showing high values, while comparatively lower values were recorded for magnesium and nickel. Nickel was the only mineral that showed positive correlation with all the minerals, as well as with leaf size and foliage yield. Zinc showed strong positive relationship with iron (0.66**) and manganese (0.74**), and was the only mineral exhibiting significant positive association with foliage yield. This study would be of use in enhancement of selected minerals in different regions according to local preferences and nutrient deficiency prevalent among the populations.

The commensal microbiota, host immunity and metabolism participate in a signalling network, with diet influencing each component of this triad. In addition to diet, many elements of a modern lifestyle influence the gut microbiota but the degree to which exercise affects this population is unclear. Therefore, we explored exercise and diet for their impact on the gut microbiota. Since extremes of exercise often accompany extremes of diet, we addressed the issue by studying professional athletes from an international rugby union squad. Two groups were included to control for physical size, age and gender. Compositional analysis of the microbiota was explored by 16S rRNA amplicon sequencing. Each participant completed a detailed food frequency questionnaire. As expected, athletes and controls differed significantly with respect to plasma creatine kinase (a marker of extreme exercise), and inflammatory and metabolic markers. More importantly, athletes had a higher diversity of gut micro-...

A new, simple and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of copper and nickel. The metals in the initial aqueous solution were complexed with 2-(2′-benzothiazolylazo)-5-(N, N-diethyl) ...

A polymerase chain reaction (PCR) was developed for the detection of Clostridium botulinum type A, a cause of human botulism. A two primer set and an oligonucleotide detection probe were used to specifically detect Cl. botulinum type A neurotoxin gene (BoNT/A). After 40 cycles of amplification, detection of a 798 bp amplified DNA fragment was carried out by agarose gel electrophoresis and Southern blot hybridization. This assay was able to detect 12.5 fg of purified target DNA or five bacteria per reaction. The sensitivity in artificially contaminated food samples after an 18 h enrichment step ranges from 10 to 10(3) bacteria per g according to the type of food samples. No cross-reactions were observed with the other Cl. botulinum toxinotypes and other bacteria found routinely in food. This PCR method may provide a suitable and rapid alternative to standard techniques for detection of Cl. botulinum type A in food samples.

In this study, 24 organochlorine pesticide residues in 109 different honey samples collected from stores and open markets in Konya, Turkey were analyzed by gas chromatography-electron capture detection. Aldrin, cis-chlordane, trans-chlordane, oxy-chlordane, 2,4′ -DDE, and 4,4′ -DDE were found in all honey samples. The mean value was 0.0540 μg g − 1 for oxy-chlordane. In the 55 samples of 109, levels of organochlorine pesticide residues of oxy-chlordane were determined as higher than those of Turkish Alimentarius Codex maximum residual limits (MRLs). Other organochlorine pesticide residues also exceeded MRLs except for cis-heptachlor epoxide and α-hexachlorocyclohexane. Since all of the honey samples are found contaminated and most of these samples exceeded MRLs, a control of organochlorine pesticide residues in honey is necessary for consumer health.

Two sensitive, selective, and precise methods for the determination of pyriproxyfen and pyridalyl insecticide residues in tomatoes have been developed. The first method is HPLC with UV detection in which pyriproxyfen and pyridalyl were extracted with ethyl acetate and acetone, respectively, followed by cleanup using column chromatography. The recoveries ranged from 86.03 to 94.55 for pyriproxyfen and 95.08 to 99.38% for pyridalyl in tomato samples. The LOD of the method was 0.217 ppm for pyriproxyfen and 0.1866 ppm for pyridalyl. The second method depends on direct fluorometric determination of pyriproxyfen and pyridalyl in acetic and sulfuric acid at excitation and emission wavelengths of 320 and 646 nm, respectively. The recoveries of pyriproxyfen and pyridalyl in tomato samples ranged from 88 to 98% and 86 to 93%, respectively. The LOD of the method was 0.146 ppm for pyriproxyfen and 0.078 ppm for pyridalyl. Both methods were applied successfully to determine residues and rate of...

The possible transfer and accumulation of novel DNA and/or proteins in food for human consumption derived from animals receiving genetically modified (GM) feed is at present the object of scientific dispute. A number of studies failed to identify GM DNA in milk, meat, or eggs derived from livestock receiving GM feed ingredients. The present study was performed in order to: (i) develop a valid protocol by PCR and multicomponent analysis for the detection of specific DNA sequences in milk, focused on GM maize and GM soybean; (ii) assess the stability of transgenic DNA after pasteurization treatment and (iii) determine the presence of GM DNA sequences in milk samples collected from the Italian market. Results from the screening of 60 samples of 12 different milk brands demonstrated the presence of GM maize sequences in 15 (25%) and of GM soybean sequences in 7 samples (11.7%). Our screening methodology shows a very high sensitivity and the use of an automatic identification of the amplified products increases its specificity and reliability. Moreover, we demonstrated that the pasteurization process is not able to degrade the DNA sequences in spiked milk samples. The detection of GM DNA in milk can be interpreted as an indicator of fecal or airborne contamination, respectively, with feed DNA or feed particles, although an alternative source of contamination, possibly recognizable in the natural environment can be suggested. Further studies, performed on a larger number of milk samples, are needed to understand the likely source of contamination of milk collected from the Italian market.