Degradation Products Research Articles

Metagenomic insights into the enhanced methane production by hydrochar at varied propionate concentrations

Propionate is a crucial intermediate product in anaerobic digestion (AD), but its degradation is thermodynamically unfavorable. Its accumulation in the AD system can significantly reduce methane production efficiency and may lead to severe acidification. The present study investigated the methane production at various propionate concentrations (15, 30 and 60 mM) with and without hydrochar and also explored the microbial shifts by metagenomic analysis. The findings revealed that higher propionate concentrations reduced methane production and propionate degradation efficiency, leading to acetate accumulation. The addition of hydrochar mitigated the inhibitory effects of increased propionate concentrations, notably reduced the lag phase by 20.13 % and enhanced the methane production rate by 138.43 % under 30 mM propionate. This also resulted in faster degradation of propionate and acetate. Hydrochar impacted the microbial communities’ functional potentials, enhancing methane metabolic potential in all conditions. Genomic-centric analysis revealed that hydrochar selectively enriched syntrophic propionate-oxidizing bacteria (SPOB) candidate MAG79 Syntrophopropionicum sp., which could participate in DIET, across different concentrations of propionate, with the most pronounced effect at 30 mM propionate. This was distinct from the dominant species in the control groups, MAG63 Syntrophosphaera sp. and MAG69 Syntrophobacteraceae sp.. Hydrochar further supported the growth of another DIET candidate MAG4 Methanosarcina mazei and increased the abundance of proposed syntrophic acetate-oxidizing bacterium (SAOBs), across all propionate concentrations. These effects collectively led to more efficient propionate degradation and methane production.

Dry Heating of Curcumin in the Presence of Basic Salts Yields Anti-inflammatory Dimerization Products.

Curcumin exerts some of its biological effects via degradation products formed by spontaneous oxidation at physiological, i.e., weakly basic, pH. Here, we analyzed products formed by dry heating of curcumin in the presence of a basic salt (sodium bicarbonate and others). Under the dry heating conditions employed, curcumin was completely consumed, yielding products entirely different from those obtained by autoxidative degradation in buffer. Bioassay-guided fractionation of the reaction mixture was used to identify and isolate compounds with anti-inflammatory activity in a cell-based assay. This provided two dimers of curcumin, dicurmins A and B, featuring a partly saturated naphthalene core that inhibited lipopolysaccharide-induced activation of NF-κB in RAW264.7 cells. Dicurmin A and B are unusual derivatives of curcumin lacking key functional moieties yet exhibit increased anti-inflammatory activity. The process of dry heating of polyphenols in the presence of a basic salt can serve as a novel approach to generating bioactive compounds.

Microbiota diversity of three Brazilian native fishes during ice and frozen storage

This study aimed to assess the bacterial microbiota involved in the spoilage of pacu (Piaractus mesopotamics), patinga (female Piaractus mesopotamics x male Piaractus brachypomus), and tambacu (female Colossoma macropomum × male Piaractus mesopotamics) during ice and frozen storage. Changes in the microbiota of three fish species (N = 22) during storage were studied through 16S rRNA amplicon-based sequencing and correlated with volatile organic compounds (VOCs) and metabolites assessed by nuclear magnetic resonance (NMR). Storage conditions (time and temperature) affected the microbiota diversity in all fish samples. Fish microbiota comprised mainly of Pseudomonas sp., Brochothrix sp., Acinetobacter sp., Bacillus sp., Lactiplantibacillus sp., Kocuria sp., and Enterococcus sp. The relative abundance of Kocuria, P. fragi, L. plantarum, Enterococcus, and Acinetobacter was positively correlated with the metabolic pathways of ether lipid metabolism while B. thermosphacta and P. fragi were correlated with metabolic pathways involved in amino acid metabolism. P. fragi was the most prevalent spoilage bacteria in both storage conditions (ice and frozen), followed by B. thermosphacta. Moreover, the relative abundance of identified Bacillus strains in fish samples stored in ice was positively correlated with the production of VOCs (1-hexanol, nonanal, octenol, and 2-ethyl-1-hexanol) associated with off-flavors. 1H NMR analysis confirmed that amino acids, acetic acid, and ATP degradation products increase over (ice) storage, and therefore considered chemical spoilage index of fish fillets.

A review of the physiological effects of microgravity and innovative formulation for space travelers.

During the space travel mission, astronauts' physiological and psychological behavior will alter, and they will start consuming terrestrial drug products. However, factors such as microgravity, radiation exposure, temperature, humidity, strong vibrations, space debris, and other issues encountered, the drug product undergo instability This instability combined with physiological changes will affect the shelf life and diminish the pharmacokinetic and pharmacodynamic profile of the drug product. Consequently, the physicochemical changes will produce a toxic degradation product and a lesser potency dosage form which may result in reduced or no therapeutic action, so the astronaut consumes an additional dose to remain healthy. On long-duration missions like Mars, the drug product cannot be replaced, and the astronaut may relay on the available medications. Sometimes, radiation-induced impurities in the drug product will cause severe problems for the astronaut. So, this review article highlights the current state of various space-related factors affecting the drug product and provides a comprehensive summary of the physiological changes which primarly focus on absorption, distribution, metabolism, and excretion (ADME). Along with that, we insist some of the strategies like novel formulations, space medicine manufacturing from plants, and 3D printed medicine for astronauts in longer-duration missions. Such developments are anticipated to significantly contribute to new developments with applications in both human space exploration and on terrestrial healthcare.

Vaterite-based in situ surface modification and process-dependent biocompatibility of laser sintered polypropylene

Polypropylene (PP) rapidly gains scientific attention as fatigue-resistant and lightweight tissue repair and implant material, while emerging laser-sintering based methods for PP processing further allow unlimited versatility of PP specimens and often reduced numbers of process steps, substituting traditional manufacturing approaches. Generally, PP is considered biocompatible for a variety of medical applications while showing superior long-term stability, however, thermoplastic processing of polypropylene may induce the formation of cytotoxic degradation products, necessitating its cytotoxicological assessment. In the present study, PP specimens have been fabricated using warm, quasi-isothermal and complementary cold, non-isothermal powder bed fusion (PBF), allowing processing PP at ambient powder bed temperature of 25 °C for minimizing thermal exposure and the formation of decomposition products. The surface of manufactured specimens has been modified with hybrid coatings consisting of mesoporous inorganic microcrystals of vaterite laden with model biomacromolecules, i.e., fluorescently labelled dextran, demonstrating the stable coating and attachment of dextran-loaded vaterite crystals independent of the applied PBF processing regime. Vaterite coating is degradable and enables the opportunity to endow the surface of PP with sustained release functionalities. Both coated and uncoated specimens demonstrated excellent biocompatibility independent of the applied processing regime, as evaluated in an ex ovo shell-less hen's egg model.

The impact of hot-air oven drying combined with Bacillus subtilis K[sbnd]C3 inoculation on quality characteristics and microbial profiles of salted shrimp paste

This study used hot-air oven drying with Bacillus subtilis KC3 inoculation to improve shrimp paste production. The fermentation rate, quality characteristics, as well as microbial profiles, were compared to those produced using sun-drying with/without inoculation. B. subtilis inoculation increased the degree of hydrolysis of shrimp paste (22.3–32.1 %) during fermentation, compared to those without inoculation (12.7–25.4 %), regardless of different drying methods (p < 0.05). The result corresponded to the faster development of shrimp paste characteristics, particularly color and browning intensity of inoculated samples when fermented for the same duration. More abundant halophilic, proteolytic, and lipolytic bacteria (p < 0.05) were also obtained in inoculated samples, confirming accelerated fermentation. Interestingly, there was no difference in proximate composition, pH, and aw among samples (p > 0.05), which were still in the range regulated by the product's standard. However, the protein and lipid degradation products such as nitrogen contents, 5′-nucleotides, free fatty acids or TBARS values, varied among samples, potentially influencing the release of desirable flavor precursors to a certain extent. The inoculation increased microbial richness and evenness/uniformity, according to next-generation sequencing analysis on microbiota profiles. Pearson's correlation also revealed that these microbiota profiles were correlated with several desirable quality characteristics to varying degrees. Thus, combining the inoculation with B. subtilis KC3 can enhance shrimp paste fermentation and quality when produced using an alternative hot-air oven while maintaining quality characteristics. The findings suggested the possibility of achieving a more efficient and consistent production process for shrimp paste.

Solubility, complexation and thermodynamics of the Tc(IV)–isosaccharinic acid system: Trends in the M(IV) series

Isosaccharinic acid (HISA, or ISA in its deprotonated form) is the main degradation product of cellulose under alkaline conditions. It can form strong complexes with radionuclides and other toxic metal ions, eventually enhancing their mobility in the context of nuclear waste repositories and other environmental systems. 99Tc is a redox-sensitive, long-lived fission product produced in high yield in nuclear reactors. The solubility of 99Tc(IV) was investigated in 0.5 M NaCl‒NaISA‒NaOH solutions with 6 ≤ pHm ≤ 12.5 and 10−6 M ≤ [ISA] ≤ 0.2 M. Complete chemical and thermodynamic models were derived on the basis of solubility data, (pe + pHm) measurements, redox speciation, and solid phase characterization. These models include the previously unreported aqueous complexes TcO(OH)(ISA)2‒ and TcO(OH)2(ISA)22−. In spite of the small size and high polarizability of the Tc4+ metal ion, the Tc(IV)-ISA complexes described in this work are significantly weaker than other ISA complexes formed with larger M4+ metal ions, i.e., Zr, Pu and U. This unexpected behavior can be possibly explained by the strong hydrolysis of Tc(IV) and corresponding stabilization of the TcO2+ moiety, which does not occur for other M(IV) systems. Thermodynamic data derived in this work can be implemented in geochemical calculations of relevance in the context of nuclear waste disposal and other environmental applications.

Rationalizing Fe-Modified TiO2 through doping, composite formation, and single-phase structuring for enhanced photocatalysis via inter- and intra-charge transfers

This study sheds light on how the properties of titanium dioxide (TiO2) are influenced when it is modified with iron (Fe), leading to the formation of Fe-doped-TiO2, Fe2O3-TiO2 composite, and single-phase FeTiO3 systems. The structural formation of the materials, oxidation state, and chemical environments of the elements are analyzed using XRD and XPS techniques. Band structures with UV–visible light driven properties and suitable redox potentials with improved recombination resistance along with an active inter- and intra-charge transfers were observed for Fe2O3-TiO2 and FeTiO3 systems. The photocatalytic efficiency was found to be superior for FeTiO3 system, degrading ∼97 and 100 % of phenol, malachite green and rhodamine B dyes in 150 min, respectively along with enhanced recyclability. Interestingly, a competitive S- and Z-scheme was predicted for Fe2O3-TiO2 composite, explaining its photocatalytic mechanism. The scavenger and total organic carbon analyses revealed the radicals driving the photocatalytic reactions and the nature of degradation products, respectively.

Full Validation and Application to Clinical Research of a High-Performance Liquid Chromatography Method for the Assessment of Urinary 3-Indoxyl Sulfate in Pediatric Patients with Hematopoietic Stem Cell Transplant.

3-indoxyl sulfate (3-IS) results from a hepatic transformation of indole, a tryptophan degradation product produced by commensal gut bacteria. The metabolite has shown promise as a biomarker of dysbiosis and clinical outcomes following hematopoietic stem cell transplant (HSCT) in adults. Nonetheless, there is a paucity of data regarding microbiome health and outcomes in the pediatric HSCT setting. We developed and thoroughly validated an affordable high-performance liquid chromatography/fluorescence detector (HPLC-FLD) method to quantify 3-IS in urine for use in the pediatric setting. Chromatographic separation was achieved on a C18 column (250 × 4.6 mm × 5 μm) with a mobile phase consisting of pH 4.0 acetic acid-triethylamine buffer and acetonitrile (88:12, v/v), eluted isocratically at 1 mL/min. 3-IS fluorescence detection was set at excitation/emission of 280 and 375, respectively. The method was fully validated according to FDA-specified limits including selectivity, linearity (0.10 to 10.00 mg/L, r2 > 0.997), intra- and inter-day accuracy, and precision. 3-IS stability was confirmed after three freeze-thaw cycles, for short- and medium-term on a benchtop and at 4 °C and for long-term up to 60 days at -20 °C. The validated method was used to quantify 3-IS in urine samples from HSCT pediatric patients.

Effect of antibiotics and antibiotic by-products on the chlorine resistance of biofilms in drinking water distribution systems

This study investigated the effects of tetracycline (TC) and sulfadiazine (SD), along with their degradation products, on biofilm chlorine resistance. The results showed that low concentrations of antibiotics and their degradation products promoted biofilm formation on tube surfaces and increased resistance to chlorine. There was a positive correlation between antibiotic levels, degradation products, and biofilm chlorine resistance within a specific concentration range. SD had a more significant impact on biofilm chlorine resistance compared to TC. The presence of both antibiotics and their degradation products in water led to an increase in biofilm chlorine resistance, especially when combined with 0.3 mg/L sodium hypochlorite. The study shows a positive association between antibiotic and degradation product concentrations and the biofilms' improved chlorine resistance, a phenomenon that could have major consequences for water treatment efforts. Additionally, higher concentrations of antibiotics and their degradation products were associated with reduced biodiversity within the biofilm. Overall, the findings suggest that the presence of antibiotics and their degradation products can influence biofilm formation, alter bacterial species composition, and enhance biofilm resistance to chlorine in drinking water distribution systems. This fresh perspective on the relationship between pharmaceutical residues and microbial communities in water systems could transform our approach to assuring water safety and combatting antimicrobial resistance.

Alterations in Choline Metabolism in Non-Obese Individuals with Insulin Resistance and Type 2 Diabetes Mellitus.

The prevalence of non-obese individuals with insulin resistance (IR) and type 2 diabetes (T2D) is increasing worldwide. This study investigates the metabolic signature of phospholipid-associated metabolites in non-obese individuals with IR and T2D, aiming to identify potential biomarkers for these metabolic disorders. The study cohort included non-obese individuals from the Qatar Biobank categorized into three groups: insulin sensitive, insulin resistant, and patients with T2D. Each group comprised 236 participants, totaling 708 individuals. Metabolomic profiling was conducted using high-resolution mass spectrometry, and statistical analyses were performed to identify metabolites associated with the progression from IS to IR and T2D. The study observed significant alterations in specific phospholipid metabolites across the IS, IR, and T2D groups. Choline phosphate, glycerophosphoethanolamine, choline, glycerophosphorylcholine (GPC), and trimethylamine N-oxide showed significant changes correlated with disease progression. A distinct metabolic signature in non-obese individuals with IR and T2D was characterized by shifts in choline metabolism, including decreased levels of choline and trimethylamine N-oxide and increased levels of phosphatidylcholines, phosphatidylethanolamines, and their degradation products. These findings suggest that alterations in choline metabolism may play a critical role in the development of glucose intolerance and insulin resistance. Targeting choline metabolism could offer potential therapeutic strategies for treating T2D. Further research is needed to validate these biomarkers and understand their functional significance in the pathogenesis of IR and T2D in non-obese populations.

Development of chemical categories for per- and polyfluoroalkyl substances (PFAS) and the proof-of-concept approach to the identification of potential candidates for tiered toxicological testing and human health assessment

Per- and Polyfluoroalkyl substances (PFAS) are a class of manufactured chemicals that are in widespread use and many present concerns for persistence, bioaccumulation and toxicity. Whilst a handful of PFAS have been characterized for their hazard profiles, the vast majority have not been extensively studied. Herein, a chemical category approach was developed and applied to PFAS that could be readily characterized by a chemical structure. The PFAS definition as described in the Toxic Substances Control Act (TSCA) section 8(a)(7) rule was applied to the Distributed Structure-Searchable Toxicity (DSSTox) database to retrieve an initial list of 13,054 PFAS. Plausible degradation products from the 563 PFAS on the non-confidential TSCA Inventory were simulated using the Catalogic expert system, and the unique predicted PFAS degradants (2484) that conformed to the same PFAS definition were added to the list resulting in a set of 15,538 PFAS. Each PFAS was then assigned into a primary category using Organisation for Economic Co-operation and Development (OECD) structure-based classifications. The primary categories were subdivided into secondary categories based on a chain length threshold (>=7 vs < 7). Secondary categories were subcategorized using chemical fingerprints to achieve a balance between total number of structural categories vs.level of structural similarity within a category based on the Jaccard index. A set of 128 terminal structural categories were derived from which a subset of representative candidates could be proposed for potential data collection, considering the sparsity of relevant toxicity data within each category, presence on environmental monitoring lists, and the ability to identify plausible manufacturers/importers. Refinements to the approach taking into consideration ways in which the categories could be updated by mechanistic data and physicochemical property information are also described. This categorization approach may be used to form the basis of identifying candidates for data collection with related applications in QSAR development, read-across and hazard assessment.

Hydrolysis kinetics of self-degradable diverters for well stimulation

Self-degradable diverters have gained increased popularity in well stimulation as an environmentally friendly and robust fluid diversion technology. As of now, limited data and conflicting information exist in the literature regarding the hydrolytic degradation rates of diverters under field-representative conditions, and knowing these rates is crucial for optimizing well stimulation designs. In this work, we systematically measured the degradation rates of commercial self-degradable diverters in aqueous solutions spanning a wide solution pH range of 0.3–13.6 and a wide temperature range of 60–110 °C. We first demonstrated that existing bottle degradation test protocols might return misleading results due to the alteration of solution pH by degradation products, and we developed a more reliable experimental protocol using buffer solutions instead. Using this procedure, we found that as the solution pH increased, the hydrolysis rate of diverters first decreased and then increased, with a minimal degradation rate at around pH = 4. Elevated temperatures yielded faster hydrolysis. The collected kinetic data fit reasonably well to a published kinetic model that was originally developed for pure polylactic acid in deionized water, with an R2 value over 0.98 for all pH and temperature conditions. This comparison suggests that the model can be more widely applied to describe the degradation kinetics of commercial diverters over broad temperature and pH ranges. The test protocol, experimental data, and kinetic analysis in this work provide important guidance on improving the efficiency of fluid diversion and well stimulation operations.

Solar-driven environmental fate of chlorinated parabens in natural and engineered water systems

Parabens are classified as emerging contaminants in global waters, and the ubiquitous emergence of their high-risk chlorinated products generated from chlorine-based wastewater disinfection has attracted increasing attention. However, rather limited information is available on their photofate after discharging into surface waters, and their degradation behavior after solar-based engineering water treatment is unclear. Herein, the reactivity of four chlorinated parabens with different photochemically produced reactive intermediates was measured. Quantitative contribution analysis in abating such compounds showed the dominance of direct photolysis in sunlit natural freshwaters. Introducing a technical solar/peroxymonosulfate (PMS) system could greatly improve the removal of chlorinated parabens. The economic analysis suggested that chlorinated parabens exhibited a minimum value of economic input as 93.41–158.04 kWh m-3 order-1 at 0.543–0.950 mM PMS. The high-resolution mass spectrometry analysis of the degradation products suggested that dechlorination, hydroxylation, and ester chain cleavage were the dominant transformation pathways during photolysis and solar/PMS treatment. Furthermore, the in silico prediction indicated severe aquatic toxicity of certain products but enhanced biodegradability. Overall, this investigation filled a knowledge gap on the reactivity of chlorinated parabens with diverse reactive transients and their quantitative contributions to the photolysis and solar/PMS treatment of emerging micropollutants in water.

Cobalt-free cathodes and silicon thin-film anodes towards high-capacity solid-state batteries

This study provides a comprehensive analysis of a novel battery system, which integrates a high-loading (∼5 mAh/cm2) cobalt-free cathode composed of lithium nickel manganese aluminum oxide (LiNi0.9Mn0.05Al0.05O2, NMA) into an all-solid-state cell for the first time. The argyrodite (Li6PS5Cl) solid electrolyte is used in conjunction with a 99 wt% silicon thin-film anode. Room temperature discharge capacities of >210 mAh/gNMA and > 170 mAh/gNMA were achieved at cycling rates of 0.05C and 0.25C, respectively. Electrochemical impedance spectroscopy measurements, taken during the first cycle detail onset of electrolyte degradation, lithiation of the silicon anode, and the change in charge transfer kinetics as a function of cell voltage. Raman, Fourier Transform Infrared, and X-ray photoelectron spectroscopy are used to identify the argyrodite degradation products that form in the catholyte on cycling, unveiling lithium carbonate as a potential source of oxygen-related degradation commonly alluded to in literature. Furthermore, high cell stack pressure, 350 MPa during fabrication, led to fracturing and pulverization of some cathode particles.

Contamination of a drug consumption room with drugs and potential risks for social health care workers

BackgroundStudies have shown that contamination of surfaces by illicit drugs frequently occurs in forensic laboratories when manipulating seized samples as well as in pharmacies and hospitals when preparing medicinal drugs. In this project, we extended these studies to a Drug Consumption Room to investigate drug levels and possible exposure of the staff members.MethodsWe investigated pre and post cleaning contamination by heroin and cocaine and their degradation products 6-monoacetylmorphine and benzoylecgonine on different surfaces (tables, counters, computers and door handles) and in the ambient air. We also collected urine and hair samples from staff members to check for potential short and long term contaminations.ResultsMedium to heavy contamination has been detected on most surfaces and door handles; as expected, air contamination was particularly high in the smoking room. Drug levels were < LOD to very low in the urine and the hair samples of staff members tested.ConclusionThe cleaning efficiency of the surfaces, carried out by staff and drug users after drug consumption, was often not satisfactory. The very low drug levels in hair indicate that acute health risks for staff members are low.

Stability-Indicating HPLC Method for Quantifying Process-Related Impurities in Fedratinib and Identification of Its Forced Degradation Products Using LC-MS/MS

Background: Pharmaceutical industry is characterized by rigorous quality standards to ensure the safety and efficacy of drugs. Despite stringent manufacturing processes, the presence of impurities or generation of degradation products (DPs) in pharmaceutical products remains a concern. This necessitates a comprehensive and systematic approach to analysis impurities and DPs. Objectives: This study deals with the optimization of the stable HPLC method for quantification of fedratinib impurities and its DPs characterization through LC-MS/MS. Method: Method optimization studies were conducted by analyzing standard solutions in various method parameters. The results noticed in every varied method condition were tabulated for finalizing the appropriate conditions for analyzing fedratinib. The mass spectral response of DPs was interpreted carefully for structural conformation of DPs. Results: The method is optimized as HIQSIL C18 (250mm×4.6mm;5µ) column employing 1.0 mL/min flow of phosphate buffer (pH 5.2) and acetonitrile in 45:65 (v/v) and 257 nm. This method elutes 5.4, 2.6, 9.2 and 3.5 min for fedratinib, impurity 1, 2 and 3 respectively. Method sensitivity was verified to be very sensitive that can evaluate up to 0.003, 0.015 and 0.004 µg/mL for impurity 1, 2 and 3 respectively. Well correlated calibration curve achieved in 50-200 µg/mL for fedratinib and 0.05-0.20 µg/mL for impurities. Various stress studies produce four stress DPs and were identified using LC-MS/MS. The molecular mass (g/mol) and formula of DPs were identified as 426 and C21H25N5O3S, 312 and C17H22N5O, 354 and C17H14N4O3S, 215 and C11H11N4O respectively for DP 1 to 4. Conclusion: The method proposed can successfully be helpful for quantifying the pharmaceutical impurities and DPs of fedratinib in bulk batch samples and formulations.

“Welcome to the jungle”: TLC-SERS to wade through real complex mixtures of synthetic dyes

The finding of numerous synthetic strategies between the 19th and 20th century fostered the production of an extensive spectrum of organic dyes for artistic and industrial applications. Shortly after, challenges emerged related to the rapid deterioration of these products. Nowadays, the characterization of coloured pieces of art produced in the first half of the XXth century is further complicated by the absence of reference materials with an unambiguous composition, which are frequently a mixture between the starting dyes and their degradations products. Here we demonstrate as Surface Enhanced Raman Spectroscopy coupled with the simplest separation technique, i.e. Thin Layer Chromatography, is able beyond to recognize several synthetic dyes also to identify their isomers and degradation products. The occasion was the study of a catalogue of dyed textile swatches, produced in 1951 by the well-known Italian industry ACNA (Azienda Coloranti Nazionali e Affini). An apparently easy task turned out to be, indeed, not at all obvious as we found out that the actual composition of the reference samples seldomly corresponded to the declared one. TLC-SERS investigation of historical textile swatches was complemented by the integration of liquid chromatography coupled with a diode array detector and high-resolution mass spectrometry (HPLC-DAD-HRMS). This approach allowed us to validate the findings of TLC-SERS and to distinctively characterise synthetic by-products and degradation markers resulting from the deterioration of the dyes.

Investigating the quality of extraction and quantification of bioactive compounds in berries through liquid chromatography and multivariate curve resolution

Berries are a rich source of natural antioxidant compounds, which are essential to profile, as they add to their nutritional value. However, the complexity of the matrix and the structural diversity of these compounds pose challenges in extraction and chromatographic separation. By relying on multivariate curve resolution alternating least squares (MCR-ALS) ability to extract components from complex spectral mixtures, our study evaluates the contributions of various extraction techniques to interference, extractability, and quantifying different groups of overlapping compounds using liquid chromatography diode array detection (LC-DAD) data. Additionally, the combination of these methods extends its applicability to evaluate polyphenol degradation in stored berry smoothies, where evolving factor analysis (EFA) is also used to elucidate degradation products. Results indicate that among the extraction techniques, ultrasonication-assisted extraction employing 1% formic acid in methanol demonstrated superior extractability and selectivity for the different phenolic compound groups, compared with both pressurized liquid extraction and centrifugation of the fresh berry smoothie. Employing MCR-ALS on the LC-DAD data enabled reliable estimation of total amounts of compound classes with high spectral overlaps. Degradation studies revealed significant temperature-dependent effects on anthocyanins, with at least 50% degradation after 7 months of storage at room temperature, while refrigeration and freezing maintained fair stability for at least 12 months. The EFA model estimated phenolic derivatives as the main possible degradation products. These findings enhance the reliability of quantifying polyphenolic compounds and understanding their stability during the storage of berry products.Graphical abstract

A plasma electrolytic oxidation coating on high-purity Mg with excellent long-term degradation performance and biocompatibility

A neutral electrolyte was used to prepare plasma electrolytic oxidation (PEO) coatings on biodegradable high-purity Mg (HP-Mg). Formation mechanism, surface morphology, and chemical compositions of the PEO coating were investigated. It was found that a porous layer formed first at the low cell voltage with an outward-growth characteristic, and then a dense layer was inward formed after the cell voltage reached the critical voltage. The main compositions of the PEO coating were MgF2, K2MgF4, KMgF3, Mg3(PO4)2, and MgO. Electrochemical measurements were carried out in simulated body fluid (SBF) at 37 °C to evaluate the long-term degradation performance. The coated HP-Mg exhibited superior degradation properties, and the coating remained intact over 180 days of degradation. During the degradation process, the pores and microcracks within the coating would gradually be filled with degradation products, enhancing the coating adhesion strength. The results of the cytotoxicity test validated the biosafety of the coating. Besides, a high-quality coating can be fabricated on the surface of biodegradable orthopedic Mg screws using this PEO treatment. The PEO coating possessed excellent degradation performance and biocompatibility, showing great potential in the practical production of biodegradable Mg implants.