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In this work, a complete study of the distribution of emerging mycotoxins in the human body has been carried out. Specifically, the presence of enniatins (A, A 1 , B, B 1 ) and beauvericin has been monitored in brain, lung, kidney, fat, liver, and heart samples. A unique methodology based on solid-liquid extraction (SLE) followed by dispersive liquid-liquid microextraction (DLLME) was proposed for the six different matrices. Mycotoxin isolation was performed by adding ultrapure water, acetonitrile, and sodium chloride to the tissue sample for SLE, while the DLLME step was performed using chloroform as extraction solvent. Subsequently, the analysis was carried out by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The proposed method allowed limits of quantification (LOQs) to be obtained in a range of 0.001-0.150 ng g -1 , depending on the tissue and mycotoxin. The precision was investigated intraday and interday, not exceeding of 9.8% of relative standard deviation. In addition, trueness studies achieved 75 to 115% at a mycotoxin concentration of 25 ng g -1 and from 82 to 118% at 5 ng g -1 . The application of this methodology to 26 forensic autopsies demonstrated the bioaccumulation of emerging mycotoxins in the human body since all mycotoxins were detected in tissues. Enniatin B (ENNB) showed a high occurrence, being detected in 100% of liver (7 ± 13 ng g -1 ) and fat samples (0.2 ± 0.8 ng g -1 ). The lung had a high incidence of all emerging mycotoxins at low concentrations, while ENNB, ENNB 1 , and ENNA 1 were not quantifiable in heart samples. Co-occurrence of mycotoxins was also investigated, and statistical tests were applied to evaluate the distribution of these mycotoxins in the human body., (© 2023. The Author(s).)

An analytical methodology based on the combination of dispersive magnetic solid-phase extraction (DMSPE) and liquid chromatography-mass spectrometry (LC-MS) is proposed to explore the occurrence of 13 mycotoxins (aflatoxins B 1 , G 1 , B 2 , and G 2 ; deoxynivalenol; T-2 toxin; ochratoxin A; HT-2 toxin; enniatins A, A 1 , B, and B 2 ; and beauvericin) and their derivatives in natural grass samples. Magnetic microparticles (Fe 3 O 4 ) coated with polypyrrole (PPy) polymer were used in DMSPE sample treatment as adsorbent phase, and Fourier-transform infrared spectroscopy, field emission scanning electron microscopy, and energy dispersive X-ray spectroscopy have been used for its characterization. The experimental parameters influencing the adsorption and desorption steps of DMSPE have been optimized. Method validation has been carried out obtaining limits of quantification between 0.07 and 92 μg kg -1 corresponding to enniatin B or A 1 and DON, respectively. A total of 83 natural grass samples from 8 dehesa farms were analysed. Enniatin B was found in all the samples (0.29 to 488 μg kg -1 concentration range) followed by enniatin B 1 (92.8% of the samples) with a 0.12-137 μg kg -1 concentration range. Moreover, co-occurrence of mycotoxins was studied and between 2 and 5 mycotoxins appeared simultaneously in 97.6% of the samples. Distribution of the contamination according to natural grass location was also investigated., (© 2023. The Author(s).)

A rapid and simple method has been developed for simultaneous determination of different classes of pesticide in different varieties of lettuce (Lactuca sativum). Lettuce samples were extracted by homogenization with acetone and partitioned into ethyl acetate-cyclohexane. Subsequent sample clean-up was not needed. Pesticide residues were determined by capillary gas chromatography with nitrogen-phosphorus detection (NPD). Confirmatory analysis of the pesticides was performed by capillary gas chromatography coupled with mass spectrometry in selected-ion-monitoring (SIM) mode. Recovery at two levels of fortification (ca. 0.05 and 0.20 mg kg(-1)) ranged from 63.9 to 118.6%, and relative standard deviations were below 9.5%. The proposed method was used to determine pesticide levels in different types of lettuce grown in soil from experimental fields.