Grapefruit (Citrus paradisi Macf.) is an important cultivar of the Citrus genus which contains a number of nutrients beneficial to human health. The objective of the present study was to evaluate changes in bioactive flavonoids, antioxidant behaviour, and in vitro cytoprotective effect of processed white and pink peels after oven-drying (45°C–60°C) and freeze-drying treatments. Comparison with fresh grapefruit peels was also assessed. Significant increases in DPPH, FRAPS, and ABTS values were observed in dried grapefruit peel samples in comparison with fresh peels, indicating the suitability of the treatments for use as tools to greatly enhance the antioxidant potential of these natural byproducts. A total of thirteen flavonoids were quantified in grapefruit peel extracts by HPLC-MS/MS. It was found that naringin, followed by isonaringin, was the main flavonoid occurring in fresh, oven-dried, and freeze-dried grapefruit peels. In vivo assay revealed that fresh and oven-dried grapefruit peel extracts (45°C) exerted a strong cytoprotective effect on SH-SY5Y neuroblastoma cell lines at concentrations ranging within 0.1–0.25 mg/mL. Our data suggest that grapefruit (Citrus paradisi Macf.) peel has considerable potential as a source of natural bioactive flavonoids with outstanding antioxidant activity which can be used as agents in several therapeutic strategies.
In this review, selected applications of CE-MS in recent years have been highlighted for the separation, detection and determination of environmental pollutants and food contaminants in selected samples. Trace analysis by CE-MS of analytes such as low molecular mass amines, nitroaromatics, alkylphosphonic acids, azo dyes, antidepressants, and antibiotic drugs, among others, in air, sediment and water samples have been reviewed. The CE-MS analysis of pesticides such as triazolopyrimidine sulphoanilides, different types of antibiotics (sulphonamides, beta-lactones, quinolones and tetracyclines) and other exogenous compounds such as acrylamide and toxic oligopeptides in food samples has also been reviewed. The review gives details on the fragmentations, where available, that the ionic species exhibit in-source and in ion trap, triple quadrupole and ToF MS analysers. A critical evaluation is also given of these recent CE-MS analytical methods for the separation, detection and determination of trace levels of such pollutants and contaminants with analytical information on the treatment of the samples, CE separation conditions, linearity ranges, LODs and recoveries from the different matrices presented.
Many recent papers and reviews have confirmed the powerful coupling between CE and MS due to efficient and selective separation in combination with selective detection allowing detailed characterization of many biomolecules. It is known that CE-MS is an increasingly used and sought after technique for analysis in different fields such as environmental science, food analysis, biotechnology, pharmaceutical analysis, biomedical science, forensic science, toxicology, and genetic analysis. CE-MS is particularly used in bio-omic applications (proteomic, metabolomic, and also genomic applications) for the determination of biomarkers, disease diagnosis, and therapeutic treatment monitoring. Biomarker qualification, clinical proteomics, and its implementation in routine clinical analysis have certain limitations associated with reproducibility and analytical robustness. However, CE-MS has been successfully used in numerous clinical applications in recent years when compared with other platforms. The main advantage lies in the availability of large comparable datasets that were all obtained by using the same procedure for sample preparation, analysis, and subsequent data evaluation. The scope of this review is to discuss the performance of CE-MS as a platform for bio-omics analysis and target-based applications focusing on quadrupole (Q), IT, and TOF analyzers, and the types of bioapplications that apply to the particular analyzers. Papers and reviews that were published in 2012 and 2013 with relevant CE-MS applications are considered in this review.
Several CE methods have been developed to achieve the chiral separation of citalopram (CIT) and its metabolites demethylcitalopram (DCIT), didemethylcitalopram (DDCIT), and citalopram N-oxide (CIT-NO). All of these compounds were present as racemic mixtures. The best method, which led to the first ever chiral screening of CIT, DCIT, DDCIT, and CIT-NO, involved the use of carboxymethyl-gamma-CD (CM-gamma-CD) and the entangled polymer hydroxypropylmethylcellulose (HPMC) as chiral and selectivity additives, respectively, in the buffer system. In an effort to improve the selectivity and sensitivity of the method, the chemical and instrumental parameters were optimized. The best conditions were short-end anodic hydrodynamic injection (6 s, 0.7 psi); as BGE pH 5, 20 mM phosphate buffer, 0.2% w/v CM-gamma-CD, 0.05% w/v HPMC; voltage of 28 kV with a ramp applied (0.4 s); cartridge temperature of 20 degrees C; detection at 205 nm. In addition, a simple and rapid achiral CE method for the determination of citalopram propionic acid (CIT-PA, the only anionic metabolite of CIT) is also reported for the first time. Prior to the electrophoretic procedure it was necessary to apply an extraction and preconcentration step to obtain analytes from the human urine samples. This was achieved using an optimized SPE process. Moreover, an innovatory experimental and statistical design approach, which involves the simultaneous evaluation of the global robustness and ruggedness effects, was applied. Both of the proposed methods proved to be very useful in the chiral pharmacokinetic screening of CIT and related metabolites in clinical human urine samples.
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