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Compound feed is particularly vulnerable to multi-mycotoxin contamination. A method for the determination of 12 mycotoxins; enniatins A, A1, B, B1; aflatoxins B1, B2, G1, G2; OTA; ZEA; T-2 and HT-2 by liquid chromatography-tandem mass spectrometry has been developed and applied for the analysis of laboratory rat commercial feeds. The method trueness was checked by recovery assays at three different spiked levels (n = 9). Recoveries ranged from 73% to 112%, and the intra-day and inter-day precision were lower than 9% and 13%, respectively. Limits of quantitation were lower than 15 μg/kg. Twenty-seven laboratory rats feed samples showed multi-contamination by at least three up to six different mycotoxins. ENNs B and B1, followed by ZEA were the most prevalent mycotoxins. T-2, HT-2, and OTA were not detected. ZEA showed the highest concentration levels reaching 492 μg/kg. The results underline the importance of implementing mycotoxin regular surveillance programs for laboratory animal feeds.

A method for the determination of seven trichothecenes, neosolaniol (NEO), diacetoxyscirpenol (DAS), deoxynivalenol (DON), nivalenol (NIV), fusarenon-X (FUS-X), 3-acetyldeoxynivalenol (3-ADON) and 15-acetyldeoxynivalenol (15-ADON), in laboratory rat feed by GC-MS/MS was developed. Sample extraction and purification was performed by an acidified mixture of acetonitrile/water (80-20% v/v). Limits of quantitation (LOQs) were between 1 and 10 μg kg(-1) for all studied trichothecenes. Eight concentration levels between the LOQ and 100 × LOQ were used for the calibration curves. Matrix-matched calibration was used for quantitation purposes to compensate the detector signal enhancement obtained for all the analytes. The method accuracy was evaluated by recovery assays at three concentration levels, 25, 50 and 100 μg kg(-1) (n = 9). Recoveries ranged from 62% to 97% and precision, expressed as intra- and inter-day relative standard deviations, was evaluated for all compounds. The validated method was successfully applied to the analysis of 35 laboratory rat feed samples showing mycotoxin contamination in 66% of the samples. DON was the most prevalent trichothecene followed by 15-ADON, NIV and 3-ADON. The maximum DON concentration reached in real samples was 2156 ± 4.3 μg kg(-1), while NEO, DAS and FUS-X were not detected in any sample. Multi-contamination by at least two mycotoxins was observed in 17% of the analysed feed samples.

Dietary exposure of the Valencian region population to lead, cadmium, inorganic arsenic (iAs), chromium, copper, tin and methylmercury (meHg) was assessed in a total diet study carried out in the region of Valencia in 2010–11. A total of 8100 food samples were collected and analysed. Occurrence data were combined with consumption data to estimate dietary exposure in adults (> 15 years of age) and young children (6–15 years of age). The estimated intake was calculated by a probabilistic approach. Average intake levels (optimistic scenario) for lead, iAs, chromium and tin were 0.21, 0.08, 1.79 and 1.87 µg kg−1 bw day−1 respectively; for Cd and meHg average intake levels were 0.77 and 0.54 µg kg–1 bw week−1, respectively, and for Cu, 1.60 mg day−1. In terms of risk characterisation, the results showed that 2.84% of the adult population may exceed the BMDL10 (benchmark dose lower confidence limit) established for Pb, which is linked to renal effects; whereas 28.01% of the young children population may...

Enniatins (ENs) are fungal secondary metabolites produced by genus Fusarium. The ENs exert antimicrobial and insecticidal effect, and has also been demonstrated cytotoxic effects on several mammalian cell lines. On the other hands, it has been proved that natural polyphenols have antioxidant effect. In this study, cell effects at low levels of exposure of four ENs (A, A(1), B and B(1)) and five polyphenols (quercetin, quercetin-3-β-D-glucoside, rutin, myricetin and t-pterostilbene) present in wine; and the cytoprotective effect of these polyphenols exposed simultaneously with ENs in Chinese Hamster Ovary (CHO-K1) cells, were studied. Cell effects were determined by the MTT test after 24 h of exposure. All ENs showed cytotoxic effect. The IC(50) obtained ranged from 4.5 ± 1.2 to 11.0 ± 2.7 µM. The concentration of polyphenols tested ranged from 5 to 50 µM. Polyphenols did not show cytotoxicity and the cytoprotective effect of polyphenols varies depending on the EN tested. The cytoprotective effect of polyphenols in CHO-K1 cells exposed to ENs was as follow: quercetin, from 24 to 84%; quercetin-3-β-D-glucoside, from 12 to 76%; rutin, from 17 to 83%; myricetin, from 16 to 92% and pterostilbene from 25 to 100%. All polyphenols protected CHO-K1 cells against EN A(1) exposure.

The enniatins (EN) are bioactive compounds of hexadepsipeptidic structure produced by several strains of Fusarium spp. The enniatin J3 (EN J3) was purified from extracts of Fusarium solani growth on solid medium of kamut, using semipreparative liquid chromatography (LC) followed by an analytical LC. The purity and the structure of the isolated compound were confirmed by electrospray ionization-mass spectrometry study-linear ion trap (ESI-MS-LIT). The pure fraction of EN J3 was utilized to study the cytotoxicity on differentiated and undifferentiated Caco-2 cells. The use of both chromatographic techniques allowed us to produce and purify 50 mg of EN J3 completely characterized with the technique of the ESI-MS-LIT. No statistically significant differences over control were detected on Caco-2 cells exposed to EN J3 at any of the concentrations used.

An approach based on solid-phase microextraction-liquid chromatography-mass spectrometry (SPME-LC-MS) has been developed for determining 12 insecticides (bromophos ethyl, chlorpyrifos methyl, chlorpyrifos ethyl, diazinon, fenoxycarb, fonofos, phenthoate, phosalone, pirimiphos methyl, profenofos, pyrazophos, and temephos) in honey. The influence of several parameters on the efficiency of the SPME was systematically investigated. Under optimal conditions, the procedure provided excellent linearity (>0.990), detection and quantification limits (between 0.001 and 0.1 microg g(-1) and between 0.005 and 0.5 microg g(-1), respectively), and precision (

The main physico-chemical, toxicological, and environmental properties of urea pesticides are summarized. General characteristics of analytical methods for residues of phenylurea herbicides (PUHs), sulfonylurea herbicides (SUHs), and Benzoylurea insecticides (BUIs) in crops, soil, and water samples, employed in the last 5 years are reviewed. Provided it is information about liquid-liquid and solid-phase extraction of the samples and clean-up steps. The applications of gas chromatography (GC), liquid chromatography (LC), and capillary electrophoresis (CE) techniques in the analysis of these compounds are exposed in tabular form and commented on. Sensitivity and instrument conditions of liquid and gas chromatographic techniques coupled to mass spectrometric detectors are outlined. The advantages and drawbacks of the analytical methods developed recently are discussed.

Graphitized Carbon Black (GCB) extractive cartridges are evaluated for on-line coupling with a C8 analytical column to determine eleven carbamates and one carboximide pesticide from spiked deionized water at the 1.2 μg/L level. Several experiments were carried out to ascertain whether GCB saturation, pesticide degradation on the surface, existence of by-pass channels, mobility among the bulk cartridge, or strong retention on the surface interfere with the determination of pesticides. Problems in on-line CGB elution are partially solved by modifying the acetonitrile/water gradient to contain a front of 100% acetonitrile for a few seconds. Eluting the same GCB cartridges off-line with dichloromethane/methanol gives recoveries higher than 77% for the selected pesticides.

The accumulation, persistence and fate of systemic pesticide aldicarb was melencholy evaluated in orange crops. The concentration of this pesticide and its two toxic metabolites, aldicarb sulfoxide and aldicarb sulfone was determined in leaves, rind and pulp of three orange varieties (Satsuma, Navelina and Clemetina de Nules) and in the top soil of the orange groves. The groves were located in two different places in the Valencia Community (Spain). The analysis showed that the aldicarb concentration was lower than those of aldicarb sulfoxide and aldicarb sulfone. In all cases, the residues persisted at least 160 days in vegetable samples and between 157 and 227 days in soil samples. Residue concentrations measured in the soil samples were highly variable but a relation with the organic matter content can be observed. The residue levels found in vegetal products were higher in leaves than in rind, and in rind than in pulp. The maximum residue values were obtained between 47 and 70 days after the a...

A procedure for the accumulation of organochiorine pesticides by reversed-phase adsorption on octadecylsilica glass microcolumns was used for the isolation and concentration from spiked distilled and natural waters. The pesticides were eluted from the octadecylsilica with light petroleum, and analyzed by gas chromatography using an electron capture detector. The average recovery was over 90% in spiked water samples at 0.1 ng/ml. The performance of the octadecylsilica when applied to the analysis of water samples were compared with the Rodier and the APHA solvent extraction methods.

Aldicarb was applied to the soil of Late Valencia orange field plots. A comparative study between four analytical methods is reported, the NPD-gas chromatography method being the best choice. The work also reports the study of accumulation and persistence of aldicarb and its biologically active metabolites in the soil, leaves and fruits (rind and pulp, separately). Residue content, at the ppb level, was found in the order leaves much greater than rind greater than pulp. Carbamate was found to accumulate mainly in its oxidized forms. Residues had reached a maximum level in about 90 days after application.