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Mycotoxins are secondary metabolites produced by filamentous fungi that usually contaminate food products. Coffee is a natural product susceptible to mycotoxin contamination. The present study evaluates the presence of nivalenol, deoxynivalenol, T-2 and HT-2 Toxin, diacetoxyscirpenol, aflatoxin B 1 , aflatoxin B 2 , aflatoxin G 1 , aflatoxin G 2 , fumonisin B 1 , fumonisin B 2 , ochratoxin A, zearalenone, enniatin A, enniatin A 1 , enniatin B, enniatin B 1 , and beauvericin in coffee samples, using liquid chromatography tandem mass spectrometry (LC-MS/MS). The results show that zearalenone was not present in any sample. In the positive samples the contents of fumonisins ranged from 58.62 to 537.45 μg/kg, emerging mycotoxins ranged from 0.10 to 3569.92 μg/kg, aflatoxins ranged from 0.25 to 13.12 μg/kg, and trichothecenes, excepting nivalenol, ranged from 5.70 to 325.68 μg/kg. Nivalenol presented the highest concentrations, from 0.40 to 25.86 mg/kg. Ochratoxin A ranged from 1.56 to 32.40 μg/kg, and five samples exceeded the maximum limit established by the European Commission.

In an effort to enforce the knowledge on mycotoxin occurrence and co-occurrence in dates and dried fruits, 228 samples purchased from Tunisian and Spanish markets were subjected to multi-mycotoxin liquid chromatography with tandem mass spectrometry (LC-MS/MS) analysis of 16 mycotoxins. At least one mycotoxin was detected in 160 samples (70%). The frequency of contaminated samples was 83%, 80%, 64%, 59% and 26% for dates, dried vine fruits, figs, apricots and plums, respectively but none of the analyzed samples contained detectable levels of fumonisins (FB1, FB2, FB3) or T-2 toxin (T2). The incidence and levels of mycotoxins varied in samples. The most prevalent mycotoxin was enniatin B (EnnB) (54%), followed by enniatinA1 (EnnA1) (36%); aflatoxins (AFs) (23%) and ochratoxin A (OTA) (22%). Thirteen samples contained AFs in levels that exceed the maximum limits established in EU legislation. The simultaneous contamination with 2–6 mycotoxins was observed in 51% of the analyzed samples. Lastly, intakes of the detected mycotoxins were calculated for average adult consumers and compared with the tolerable daily intakes (TDI). Data obtained were used to estimate the potential exposure levels.

In this study, 72 samples of follow-up infant formula of Spanish origin were analyzed for the presence of the mycotoxins beauvericin (BEA), enniatins (ENs) (A, A1, B, B1), and fusaproliferin (FUS). The samples analyzed were extracted three times with ethyl acetate and then the mycotoxins were identified and quantified using a liquid chromatography (LC) coupled to a diode array detector (DAD). The positive samples analyzed in this study were digested through a simulated gastrointestinal digestion model, which permit to simulate the physiological condition of the human gastrointestinal tract (duodenal and colonic compartments) in order to assess the bioaccessibility of the bioactive compounds contained in the follow-up infant formula, and to perform the approach to the risk assessment related to the intake of these bioactive compounds. The EN B, was detected in 12 of the totally positive samples with a mean value of 32.3 ± 1.2 mg/kg, whereas the EN A was evidenced only in one sample with a value of 149.62 ± 2.36 mg/kg. The EN A1 presented a mean contamination of 55.36 ± 2.1 mg/kg. The duodenal bioaccessibility of the bioactive compounds present in the analyzed samples ranged from 0.37 to 22.41%, whereas employing the duodenal + colonic digestion the mean bioaccessibility of the mycotoxins studied ranged from 1.63 to 29.00%.

The occurrence of enniatins (ENs) and beauvericin (BEA) in nuts, dried fruits and dates available in Valencia (Spain) was surveyed in this study. To do this, seventy-four samples of nuts, dried fruits and dates were analyzed for the determination of mycotoxin contamination. Mycotoxins were identified and quantified using an ultrasonic-C18 extraction and LC–MS/MS with a triple quadrupole (QqQ) mass analyzer. The frequencies of contamination of nuts, shell, dried fruits and dates were 50%, 80%, 35.7% and 83.3%, respectively. Enniatin A (ENA) was the most predominant EN found in nuts (45.2%) while ENB was the most common EN found in dates (58.3%). The analytical results of the shell samples showed a protective effect of the shell, avoiding the contamination of the fruit with mycotoxins.

A new rapid, sensitive, reproducible and reliable method was developed for the quantitative determination of enniatins A, A1, B and B1, beauvericin and fusaproliferin in dry and fresh pasta by liquid chromatography-triple quadrupole-tandem mass spectrometry. A comparative study of different rapid and economical extraction procedures was performed for the extraction of these mycotoxins in pasta. For this purpose, three different approaches were studied during the extraction step (Ultra-Turrax, ultrasonic bath and microwave). Optimal extraction conditions were reached using Ultra-Turrax with acetonitrile for 3 min without purification step. The chromatographic separation of the six mycotoxins was accomplished in 15 min. The method was extensively validated with satisfactory results: recovery rates ranged from 86 to 112% and the relative standard deviations were lower than 15%. Limits of detection ranged from 0.02 to 0.15 μg kg−1. The applicability of the method was assessed with the analysis of 30 samples of dry and fresh pasta.

Forty-five samples of Spanish follow-up infant formula with different chemical compositions were analyzed determining the emerging Fusarium mycotoxins beauvericin (BEA), enniatins (ENs) (A, A 1 , B, B 1 ), and fusaproliferin (FUS). The samples were extracted three times with ethyl acetate using an Ultra-turrax homogenizer. Mycotoxins were identified and quantified using a liquid chromatography (LC) coupled to a diode array detector (DAD). Results showed that the percentage of the samples contaminated with ENs and FUS were 46.6 and 20.0% respectively, whereas all analyzed samples were free of BEA. The ENs A and B were detected only in one sample with 149.6 and 39.4 mg/kg respectively. The ENB 1 was the more detected mycotoxin with levels ranging from 11.4 to 41.9 mg/kg. The ENA 1 was detected at levels ranging from 6.3 to 101.7 mg/kg. The minor Fusarium mycotoxin FUS was detected in a range variable from 0.7 to 1.7 mg/kg. Finally, dietary exposure of Spanish infants (between 6 and 12 months) to ENs, BEA and FUS, was estimated through the consumption of commercial follow-up infant formula by the calculation of the estimated daily intake (EDI). Considering the sum of the mycotoxins studied, the data evidenced that the EDI was 236.2 μg/kg bw/day.

In this study, 64 samples of raw cereals (wheat, maize and barley) purchased from local markets in Rabat–Sale area from Morocco were analyzed for the occurrence of six emerging mycotoxins: four enniatins ENs (ENA, ENA1, ENB and ENB1), beauvericin (BEA) and fusaproliferin (FUS). Samples were extracted with a mixture of water/acetonitrile (85/15, v/v) by using an Ultra-turrax homogenizer. Mycotoxins were then identified and quantified with a liquid chromatography (LC) with diode array detector (DAD). Positive samples were confirmed with an LC–MS/MS. Analytical results showed that the frequencies of contamination of total samples with ENs, BEA and FUS were 50, 26.5 and 7.8%, respectively. ENA1 was the most common EN found with a percentage of contamination of 39%, levels ranged between 14 and 445 mg/kg. ENB contaminated 14 samples (21.8%) and levels ranged from 5 to 100 mg/kg. ENB1 was present in four samples (6.2%) and levels varied from 8 to 32 mg/kg. ENA was detected in only one sample with 34 mg/kg. BEA levels ranged from 1 to 59 mg/kg and FUS levels varied from 0.6 to 2 mg/kg. The present report is the first one ever drafted on the presence of emerging Fusarium mycotoxins in raw cereals available in Morocco.

A total of 155 samples, including meat and milk, were analyzed using a method developed for determining five macrolide antibiotics: tilmicosin (TILM), tylosin (TS), spiramycin (SPM), erythromycin (ERY), and tulathromycin (TULA) and two lincosamide antibiotics: pirlimycin (PIRL) and lincomycin (LM). The method was performed by pressurised liquid extraction (PLE) coupled to LC–MS/MS using electrospray ionization in positive ion mode. 2.5 mL of milk or 2.5 g of meat were dispersed in ethylenediaminetetraacetic acid sodium salt 2-hydrate (EDTA) and sea sand. The PLE conditions as: solvent, temperature, pressure, static time, and cell size were optimized. The following analytical parameters were validated according to the guidelines laid down by European Commission Decision 2002/657/EC linearity, specificity, decision limit (CCα), detection capability (CCβ), repeatability, reproducibility, recovery and ruggedness. The frequency of analyzed antibiotics in milk and meat was 48 and 15%, respectively. Four of positives samples (two of meat and two of milk) were higher than the maximum residues levels (MRLs) established by European Union legislation. The found levels were lower than 78.3 μg/kg in milk and 156 μg/kg in meat. Calculation of the estimated daily intakes (EDIs) from these data showed that contribution of meat and milk to dietary intakes were lower than acceptable daily intakes (ADIs) proposed by JECFA.

A method for determination of zearalenone in cereal flour has been developed applying pressurized liquid extraction (PLE) using methanol/acetonitrile (50:50 v/v) as the extraction solvent. The extracted samples were analyzed with liquid chromatography coupled to mass spectrometry (LC–MS) with an electro spray ionisation interface (ESI). The method was validated as a quantitative confirmatory method according to the Eu Commission Decision 2002/657/EC. Recoveries of the extraction step data were satisfactory with values higher then 70%. Quantification limits (LOQ) were 5 μg/kg for ESI (+) and 1 μg/kg for ESI (−). Twenty one flour samples produced in different countries were extracted and analyzed by LC–MS (ESI) negative ionisation followed by LC–MS (ESI) positive ionisation for confirmative purposes, quantification was based on matrix-matched standard curves to compensate disturbing matrix effect. Only one sample was confirmed containing zearalenone below levels regulated by European Commission.

The aim of this study was to investigate the pesticide residues in market fruits (oranges, tangerines, nectarines, peaches and khakis) from one Valencian Cooperative (Spain) and to conduct a monitoring of 32 organophosphorous, organonitrogen and organohalogenated pesticides and nine dithiocarbamate fungicides (DTCFs) usually applied on cultures of this area. Extracts were obtained by an official procedure for routine analysis based on ethyl acetate extraction. Residues of pesticides were determined by gas chromatography with nitrogen phosphorous detector (NPD), electron-capture detector (ECD) and mass spectrometry (MS) detectors. Mean recoveries obtained at fortification levels between 0.05 and 5 mg kg−1 were in range of 56–97% with relative standard deviations (RSDs) from 5% to 18%. The limits of quantification (LOQs) were in range of 0.1–140 μg kg−1 and lower than maximum residue limits (MRL) established by the Spanish legislation. 73% of the samples had no detectable residues. Of the contaminated samples, 13.8% exceeded the maximum residue limits (MRLs). Peaches and oranges showed the lowest contamination rates (13.9% and 21.3%, respectively). The contamination and violation rates were similar than the percentages recorded in previous monitoring studies in the same Community. Estimated daily intakes (EDIs) were calculated for these compounds in basis of European maximum residue limits (MRL) and residues found in the analysed samples and were compared with the acceptable daily intakes (ADIs).

One hundred and sixteen orange and tangerine samples from an agricultural cooperative of the Valencian Community (Spain) were analyzed for bitertanol, carbendazim, hexythiazox, imazalil, imidacloprid, methidathion, methiocarb, pyriproxyfen, thiabendazole, and trichlorfon by liquid chromatography–mass spectrometry (LC–MS) after a conventional multiresidue extraction procedure. Of 52 samples that contained pesticide residues, carbendazim was detected in 27 (51.9%) in the concentration range of 0.02–0.04 mg kg−1, hexythiazox in 22 (42.3%) in the concentration range of 0.02–0.05 mg kg−1, imazalil in 8 (15.0%) in the concentration range of 0.02–1.2 mg kg−1, imidacloprid in 5 (9.6%) in a concentration range of 0.02–0.07 mg kg−1 methidathion in 17 (32.6%) in the concentration range of 0.06–1.3 mg kg−1, and methiocarb in 1 (2%) at a concentration of 0.02 mg kg−1. Bitertanol, pyriproxyfen, thiabendazole and trichlorfon were not detected in any sample. Although 19 samples contained residues of two or three of the studied pesticides, no sample exceeded the European Maximum Residue Limits (MRLs). The results show that despite a high occurrence of pesticide residues in oranges and tangerines from Valencian Community, the contamination levels of these residues could not be considered a serious public health problem according to European Union (EU) regulations.