Application of capillary electrophoresis-mass spectrometry for determining organic food contaminants and residues

Food contamination continues to be a serious problem around the world. Surveillance of chemical contaminants in foods is important not only for public health but also because of the negative economic impact of contamination. From the analytical perspective, analysis of contaminants in food is an extremely challenging area. There is a wide variety of questions, ranging from the quantification of extremely low levels of individual components to the detailed assessment and evaluation of the analytical technique possibilities. This review considers the applications of CE coupled to MS detection (CE-MS) for the analysis of organic contaminants in food. Analytical information on sample concentration techniques, as well as on the CE separation conditions and recoveries obtained from water and food are provided. Different sections include several fields of application, such as pesticides, drug residues, or toxic formed during food processing in different matrices. A number of tables report a comprehensive listing of CE-MS applications. As a result, this work presents an update overview on the principal application of CE-MS together with a discussion of their main advantages and drawbacks, and an outline of future trends on analysis of organic contaminants.     

Sediment extraction and clean-up for organic phosphorus analysis by electrospray ionization tandem mass spectrometry

A method to prepare NaOH sediment extracts for organic P compound analysis with electrospray ionization tandem mass spectrometry (ESI-MS-MS) was developed on natural samples. Ion exchange, rotary evaporation and mass cut-off filtering proved to be suitable for sample preparation. Samples were analyzed with ESI-MS-MS, and reproducibility and repeatability of the method was calculated. In addition, ³¹P-nuclear magnetic resonance spectroscopy (³¹P NMR) was used to measure recovery of different P compound groups such as orthophosphate (Ortho-P), orthophosphate monoesters (Monoester-P), orthophosphate diesters (Diester-P) and pyrophosphates (Pyro-P).

The developed sample preparation method resulted in an easy-to-spray liquid for the ESI-MS-MS instrumentation. The overall P recovery was 65% and ³¹P NMR showed that Diester-P, possibly in the form of DNA, was apparently lost through the filtering step most likely due to their size. Variances in the total intensities of the MS scans (relative standard deviation (R.S.D.) 35–54%) were for about 50% due to repeated MS runs. Covariances of the peaks in the MS spectra were calculated to be for about 30% due to the sample preparation procedure. Finally, with the ESI-MS-MS approach, 11 peaks in the mass spectra were found likely to represent phosphate containing compounds.     

Serinolic amino-s-triazines: iterative synthesis and rotational stereochemistry phenomena as N-substituted derivatives of 2-aminopropane-1,3-diols

The iterative synthesis of 2,4,6-triamino-s-triazines (melamines), precursors and dendritic structures, by amination of cyanuric chloride with C-1 versus C-2-substituted 2-aminopropane-1,3-diols (serinols), is comparatively examined. The stereochemistry of the resulting serinolic amino-s-triazines, issued from the restricted rotation about the newly created C(s-triazine)-N bonds, is for the first time discussed in terms of (pro)diastereomerism based on DNMR and DFT calculation data.     

Anti-inflammatory Glycocalyx-Mimicking Nanoparticles for Colitis Treatment: Construction and In Vivo Evaluation

Common medications for treating inflammatory bowel disease (IBD) have limited therapeutic efficacy and severe adverse effects. This underscores the urgent need for novel therapeutic approaches that can effectively target inflamed sites in the gastrointestinal tract upon oral administration, exerting potent therapeutic efficacy while minimizing systemic effects. Here, we report the construction and in vivo therapeutic evaluation of a library of anti-inflammatory glycocalyx-mimicking nanoparticles (designated GlyNPs) in a mouse model of IBD. The anti-inflammatory GlyNP library was created by attaching bilirubin (BR) to a library of glycopolymers composed of random combinations of the five most naturally abundant sugars. Direct in vivo screening of 31 BR-attached anti-inflammatory GlyNPs via oral administration into mice with acute colitis led to identification of a candidate GlyNP capable of targeting macrophages in the inflamed colon and effectively alleviating colitis symptoms. These findings suggest that the BR-attached GlyNP library can be used as a platform to identify anti-inflammatory nanomedicines for various inflammatory diseases.     

Enantioselective Catalytic Addition of N-Acyl Radicals: In Batch and In Flow Organophotoredox α-Amination of Aldehydes

The organophotoredox catalytic enantioselective addition of N-acyl radicals to aldehydes, to afford enantioenriched N-acyl 1,2 aminoalcohols was studied. Under the best conditions, in batch, the product was isolated in up to 52 % yield and 85 % e.e., using a low cost and commercially available chiral imidazolidinone as organocatalyst. The reaction was then studied in flow, exploring different experimental setups and photoreactors. Although modest yields were obtained, the in-flow process afforded the product in higher productivities (up to 60 times higher) and improved space time yields (increased up to 113 times) compared to the batch reaction, with no loss of stereoselectivity.     

An echolocation visualization and interface system for dolphin research

The present study describes the development and testing of a tool for dolphin research. This tool was able to visualize the dolphin echolocation signals as well as function as an acoustically operated "touch screen." The system consisted of a matrix of hydrophones attached to a semitransparent screen, which was lowered in front of an underwater acrylic panel in a dolphin pool. When a dolphin aimed its sonar beam at the screen, the hydrophones measured the received sound pressure levels. These hydrophone signals were then transferred to a computer where they were translated into a video image that corresponds to the dynamic sound pressure variations in the sonar beam and the location of the beam axis. There was a continuous projection of the image back onto the hydrophone matrix screen, giving the dolphin an immediate visual feedback to its sonar output. The system offers a whole new experimental methodology in dolphin research and since it is software-based, many different kinds of scientific questions can be addressed. The results were promising and motivate further development of the system and studies of sonar and cognitive abilities of dolphins.     

Statistical independence in nonlinear maps coupled to non-invertible transformations

We investigate the connections between functions of type xn=p(θTzn) and nonlinear maps coupled to non-invertible transformations. These systems can produce unpredictable dynamics. We study the higher-order correlations in the generated sequences. We show that (theoretically) it is possible to construct systems that can generate sequences that constitute a set of statistically independent random variables. We apply the results in the improvement of a two-dimensional coupled map system that has been used in practical applications as e.g. cryptosystems and data compression.     

Silibinin and Naringenin against Bisphenol A-Induced Neurotoxicity in Zebrafish Model—Potential Flavonoid Molecules for New Drug Design,Development, and Therapy for Neurological Disorders

Bisphenol A (BPA), a well-known xenoestrogen, is commonly utilised in the production of polycarbonate plastics. Based on the existing evidence, BPA is known to induce neurotoxicity and behavioural issues. Flavonoids such as silibinin and naringenin have been shown to have biological activity against a variety of illnesses. The current research evaluates the neuropharmacological effects of silibinin and naringenin in a zebrafish model against neurotoxicity and oxidative stress caused by Bisphenol A. In this study, a novel tank diving test (NTDT) and light–dark preference test (LDPT) were used in neurobehavioural investigations. The experimental protocol was planned to last 21 days. The neuroprotective effects of silibinin (10 μM) and naringenin (10 μM) in zebrafish (Danio rerio) induced by BPA (17.52 μM) were investigated. In the brine shrimp lethality assay, the 50% fatal concentrations (LC₅₀) were 34.10 μg/mL (silibinin) and 91.33 μg/mL (naringenin) compared to the standard potassium dichromate (13.15 μg/mL). The acute toxicity investigation found no mortality or visible abnormalities in the silibinin- and naringenin-treated groups (LC₅₀ > 100 mg/L). The altered scototaxis behaviour in LDPT caused by BPA was reversed by co-supplementation with silibinin and naringenin, as shown by decreases in the number of transitions to the light zone and the duration spent in the light zone. Our findings point to BPA’s neurotoxic potential in causing altered scototaxis and bottom-dwelling behaviour in zebrafish, as well as the usage of silibinin and naringenin as potential neuroprotectants.     

Detection of biliary complications after orthotopic liver transplantation with MR cholangiography.

To assess the diagnostic value of magnetic resonance cholangiography (MRC) when evaluating biliary complications in the follow-up of liver transplant patients. One hundred and thirteen patients prospectively underwent MR imaging and MR cholangiography at 1.5-T unit after orthotopic liver transplantation (OLT). After the acquisition of axial T1- and T2-weighted sequences, MRC involved a coronal, non breath-hold, respiratory-triggered, fat-suppressed, two-dimensional, thin-slab, heavily T2-weighted fast spin-echo sequence, and coronal breath-hold, thick-slab, single-shot T2-weighted sequences. The images and maximum intensity projections were evaluated by two readers in order to determine biliary anatomy and the presence of complications, whose final diagnosis was based on endoscopic retrograde cholangiography (ERC) in 50 patients, percutaneous trans-hepatic cholangiography (PTC) in five, and by integrating clinical follow-up with ultrasound and MR findings in 58 cases. MRC had a sensitivity of 93%, a specificity of 92%, a positive predictive value of 86%, a negative predictive value of 96%, and a global diagnostic accuracy of 93% in detecting all types of biliary complications in OLT patients. MRC is a reliable technique for detecting post-OLT biliary complications. We now restrict the use of ERC to patients for whom therapeutic procedures are advocated or whose MRC results are equivocal.     

Analysis of Pros and Cons in Using [68Ga]Ga-PSMA-11 and [18F]PSMA-1007: Production,Costs, and PET/CT Applications in Patients with Prostate Cancer

The aim of this work is to compare [⁶⁸Ga]Ga-PSMA-11 and [¹⁸F]PSMA-1007 PET/CT as imaging agents in patients with prostate cancer (PCa). Comparisons were made by evaluating times and costs of the radiolabeling process, imaging features including pharmacokinetics, and impact on patient management. The analysis of advantages and drawbacks of both radioligands might help to make a better choice based on firm data. For [⁶⁸Ga]Ga-PSMA-11, the radiochemical yield (RCY) using a low starting activity (L, average activity of 596.55 ± 37.97 MBq) was of 80.98 ± 0.05%, while using a high one (H, average activity of 1436.27 ± 68.68 MBq), the RCY was 71.48 ± 0.04%. Thus, increased starting activities of [⁶⁸Ga]-chloride negatively influenced the RCY. A similar scenario occurred for [¹⁸F]PSMA-1007. The rate of detection of PCa lesions by Positron Emission Tomography/Computed Tomography (PET/CT) was similar for both radioligands, while their distribution in normal organs significantly differed. Furthermore, similar patterns of biodistribution were found among [¹⁸F]PSMA-1007, [⁶⁸Ga]Ga-PSMA-11, and [¹⁷⁷Lu]Lu-PSMA-617, the most used agent for RLT. Moreover, the analysis of economical aspects for each single batch of production corrected for the number of allowed PET/CT examinations suggested major advantages of [¹⁸F]PSMA-1007 compared with [⁶⁸Ga]Ga-PSMA-11. Data from this study should support the proper choice in the selection of the PSMA PET radioligand to use on the basis of the cases to study.