Determination of zearalenone and its metabolites in endometrial cancer by coupled separation techniques

This study presents a selective method of isolation of zearalenone (ZON) and its metabolite, α-zearalenol (α-ZOL), in neoplastically changed human tissue by accelerated solvent and ultrasonic extractions using a mixture of acetonitrile/water (84/16% v/v) as the extraction solvent. Extraction effectiveness was determined through the selection of parameters (composition of the solvent mixture, temperature, pressure, number of cycles) with tissue contamination at the level of nanograms per gram. The produced acetonitrile/water extracts were purified, and analytes were enriched in columns packed with homemade molecularly imprinted polymers. Purified extracts were determined by liquid chromatography (LC) coupled with different detection systems (diode array detection - DAD and mass spectrometry - MS) involving the Ascentis RP-Amide as a stationary phase and gradient elution. The combination of UE-MISPE-LC (ultrasonic extraction - molecularly imprinted solid-phase extraction - liquid chromatography) produced high (R ≈ 95–98%) and repeatable (RSD < 3%) recovery values for ZON and α-ZOL

Disentangling the heterogeneity of autism spectrum disorder through genetic findings

Autism spectrum disorder (ASD) represents a heterogeneous group of disorders, which presents a substantial challenge to diagnosis and treatment. Over the past decade, considerable progress has been made in the identification of genetic risk factors for ASD that define specific mechanisms and pathways underlying the associated behavioural deficits. In this Review, we discuss how some of the latest advances in the genetics of ASD have facilitated parsing of the phenotypic heterogeneity of this disorder. We argue that only through such advances will we begin to define endophenotypes that can benefit from targeted, hypothesis-driven treatments. We review the latest technologies used to identify and characterize the genetics underlying ASD and then consider three themes—single-gene disorders, the gender bias in ASD, and the genetics of neurological comorbidities—that highlight ways in which we can use genetics to define the many phenotypes within the autism spectrum. We also present current clinical guidelines for genetic testing in ASD and their implications for prognosis and treatment

Analysis of alternariol and alternariol monomethyl ether in foodstuffs by molecularly imprinted solid-phase extraction and ultra-high-performance liquid chromatography tandem mass spectrometry

Molecularly imprinted porous polymer microspheres selective to Alternaria mycotoxins, alternariol (AOH) and alternariol monomethyl ether (AME), were synthesized and applied to the extraction of both mycotoxins in food samples. The polymer was prepared using 4-vinylpiridine (VIPY) and methacrylamide (MAM) as functional monomers, ethylene glycol dimethacrylate (EDMA) as cross-linker and 3,8,9-trihydroxy-6H-dibenzo[b, d] pyran-6- one (S2) as AOH surrogate template. A molecularly imprinted solid phase extraction (MISPE) method has been optimized for the selective isolation of the mycotoxins from aqueous samples coupled to HPLC with fluorescence (lambda(ex)= 258 nm;lambda(em) = 440 nm) or MS/MS analysis. The MISPE method was validated by UPLC-MS/MS for the determination of AOH and AME in tomato juice and sesame oil based on the European Commission Decision 2002/657/EC. Method performance was satisfactory with recoveries from 92.5% to 106.2% and limits of quantification within the 1.1-2.8 mu g kg(-1) range in both samples

Facile preparation of carbon nanotube-based molecularly imprinted monolithic stirred unit

A lab-made stirring extraction unit based on a selective monolithic solid was developed. The monolith was formed by interconnected carbon nanotubes which were covered by a thin polymeric layer, where specific cavities were generated to provide selective recognition sites in the material. To reach this goal, a water-in-oil (W/O) medium internal phase emulsion (40/60 w/w%), was prepared and photopolymerized. The polymerization reaction took place in the organic or external phase containing the carbon nanotubes, polymeric monomers (cross-linker and functional monomer) and a molecule template. Therefore, it was possible to coat the nanotubes with a layer of molecularly imprinted polymer (MIP) with the target analyte while forming a monolithic and macroscopic structure. The developed selective monolithic stirring extraction units were applied for the determination of secbumeton and structurally related compounds (triazine herbicides) in peppermint mint and tea samples. Their adsorption capacity and selectivity were also compared with a non-imprinted polymer (NIP). Finally, the performance of the method was evaluated for quantitative analysis, achieving limits of detection (LODs) between 0.4 and 2.5 μg·L−1. The intra- and inter-day precision of the method was also evaluated as relative standard deviation, observing values which ranged from 3% to 9% and 9% to 15%, respectively