Aqueous Research Articles

Limitations of Limulus amebocyte lysate test for endotoxin control in raw materials for liposomal nanoformulations.

Aim: To evaluate the applicability of Limulus amebocyte lysate (LAL) assay for endotoxin determination in lipid compounding liposomal nanoformulations.Materials & methods: Spiked cholesterol, hydrogenated soy phosphatidylcholine and 1,2-distearoyl-sn-glycero-3-phosphoethanolamine-N-[amino(polyethylene glycol)-2000] (DSPE-PEG 2000) samples with endotoxins, simulating contaminated samples or in-process contamination were analyzed by chromogenic LAL assay.Results: Recovery of spiked endotoxins was achieved from DSPE-PEG 2000 suspended in water, whereas recovery was not achieved from spiked cholesterol and hydrogenated soy phosphatidylcholine suspended in methanol, and from multilamellar vesicles. Conclusion: Endotoxins, when in contact with organic solvents, no longer react in the LAL assay as they do in aqueous media. This indicates limitations of the LAL assay for endotoxin control in raw materials for liposomal nanoformulations.

N-Substituted Iminothiolane (NIT): A Promising Strategy for Protecting Lysine Side Chains for Solid-Phase Peptide Chemistry.

In this study, we introduce N-substituted iminothiolane (NIT) as a robust protecting group for lysine side chains. NIT is compatible with Fmoc-SPPS and can be efficiently removed under mild nucleophilic conditions. Notably, NIT offers enhanced hydrophilicity compared to traditional orthogonal lysine-protecting groups and does not undergo intramolecular migration. Additionally, the synthesis of NIT in aqueous media highlights its eco-friendly nature, positioning it as a promising alternative to protect lysine side chains.

Impact of dehulling, germination and fermentation on the bioactive and functional properties of grey pea flour

IntroductionGrey pea is a largely overlooked legume in the Nordic countries, and its potential uses in various food products remain unexplored. It is a nutrient-rich crop with low environmental impact, making it an attractive option for sustainable and nutritious plant-based alternatives.ObjectivesTo investigate the impact of dehulling, germination, and fermentation on the bioactive (polyphenol content and antioxidant capacity) and functional characteristics (water absorption index, water solubility index, water and oil binding capacity, emulsifying properties and gelation concentration) of grey pea flour. Additionally, protein content and pasting properties (temperature, peak viscosity, trough viscosity, breakdown, final viscosity, and setback) were measured.MethodsDehulling was performed using a runner disk sheller. Germination was carried out for 24 and 48 h at ambient temperature, and fermentation was conducted for 8 h at 43°C using a starter culture.ResultsThe results indicate that dehulling did not significantly affect functional properties and gelling capacity (p = 0.297 for oil absorption capacity, p = 0.5 for emulsion activity, and p = 0.607 for emulsion stability), but it resulted in a notable decrease in total polyphenol content (TPC) and antioxidant capacity (TAC). Conversely, 48 h of germination increased TAC measured by two methods: FRAP (19%) and DPPH (30%). This process increased through viscosity by 1.2-fold, while it did not significantly affect the water absorption index (WAI), water solubility index (WSI), or the emulsifying properties of grey pea flour. Fermentation significantly improved TPC (p < 0.001 for whole grey peas and p = 0.004 for dehulled grey peas), with a TPC increase of up to 67% in fermented dehulled pea flour. TAC measured by both methods, showed significant increases, ranging from 35 to 104%. However, fermentation reduced emulsifying and pasting properties, as indicated by the peak, through and final viscosity, which may be desirable only for certain food products. Further, germination and fermentation showed significant increases in protein content, by 4 and 8%, respectively.ConclusionFermented grey pea flour exhibited enhanced bioactive characteristics, while 48-h germination positively impacted pasting properties. Overall, these processes led to changes in both the bioactive and functional properties of grey pea flour, creating opportunities for the use of these flours in a wide array of food products.

Camptothecin and its derivatives: Advancements, mechanisms and clinical potential in cancer therapy.

Camptothecin (CPT), an alkaloid isolated from the Camptotheca tree, has demonstrated significant anticancer properties in a range of malignancies. However, its therapeutic efficacy is limited by its hydrophobicity, poor bioavailability, and systemic toxicity. Derivatives, analogues, and nanoformulations of CPT have been synthesized to overcome these limitations. The aim of this review is to comprehensively analyze existing studies to evaluate the therapeutic efficacy, mechanistic aspects, and clinical potential of CPT and its modified forms, including derivatives, analogues, and nanoformulations, in cancer treatment. A comprehensive literature review was performed using PubMed/Medline, Scopus, and Web of Science databases; articles were selected based on specific inclusion criteria, and data were extracted on the pharmacological profile, clinical studies, and therapeutic efficacy of CPT and its different forms. Current evidence suggests that derivatives and analogues of CPT have improved water solubility, bioavailability, and reduced systemic toxicity compared to CPT. Nanoformulations further enhance targeted delivery and reduce off-target effects. Clinical trials indicate promising outcomes with enhanced survival rates and lower side effects. CPT and its modified forms hold significant promise as potent anticancer agents. Ongoing research and clinical trials are essential for establishing their long-term efficacy and safety; the evidence overwhelmingly supports further development and clinical testing of these compounds.

Upgrading Isoquercitrin Concentration via Submerge Fermentation of Mulberry Fruit Extract with Edible Probiotics to Suppress Gene Targets for Controlling Kidney Cancer and Inflammation.

In recent years, kidney cancer has become one of the most serious medical issues. Kidney cancer is treated with a variety of active compounds that trigger genes that cause cancer. We identified in our earlier research that isoquercitrin (IQ) can activate PIK3CA, IGF1R, and PTGS2. However, it has a very low bioavailability because of its lower solubility in water. So, we utilized sub-merge fermentation technology with two well-known probiotics, Lactobacillus acidophilus and Bacillus subtilis, as a microbial source and mulberry fruit extract as a substrate, which has a high IQ level to improve IQ yield. Furthermore, we compared the total phenolic, flavonoid, and antioxidant contents of fermented and non-fermented samples, and we found that the fermented samples had greater levels than non-fermented sample. In addition, the high-performance liquid chromatography (HPLC) results showed that the fermented mulberry fruit extract from B. subtilis and L. acidophilus showed higher IQ values (190.73 ± 0.004μg/ml and 220.54 ± 0.007μg/ml, respectively), compared to the non-fermented samples, which had IQ values (80.12 ± 0.002μg/ml). Additionally, at 62.5µg/ml doses of each sample, a normal kidney cell line (HEK 293) showed higher cell viability for fermented and non-fermented samples. Conversely, at the same doses, the fermented samples of L. acidophilus and B. subtilis in a kidney cancer cell line (A498) showed an inhibition of cell growth around 36% and 31%, respectively. Finally, we performed RT and qRT PCR assay, and we found a significant reduction in the expression of the PTGS2, PIK3CA, and IGF1R genes. We therefore can conclude that the fermented samples have a higher concentration of isoquercitrin, and also can inhibit the expression of the genes PTGS2, PIK3CA, and IGF1R, which in turn regulates kidney cancer and inflammation.

Microwave‐Assisted, Multicomponent Synthesis of Pyrazolo [3, 4‐b] Pyridines Under Green Conditions

AbstractDeveloping novel and environmentally friendly green methodologies are critical in synthetic organic chemistry. Here, we investigated the one‐pot, efficient green synthesis of pyrazolo[3,4‐b]pyridine derivatives via a multicomponent approach. The reactions were operated in an aqueous medium by using microwave irradiation and conventional protocols. The green protocol offered high yields of desired product in swift reaction time, and good tolerance under reaction conditions.

Separation of no-carrier-added Bi and stable Bi from thallium

Abstract No carrier added 204,206Bi radioisotopes were produced by alpha induced reaction on Tl2CO3 target. Liquid liquid extraction method using 18-crown-6 dissolved in nitrobenzene and HClO4 was developed for the separation of NCA 204,206Bi from bulk Tl target. Bulk Tl was observed to be extracted by the organic phase at higher HClO4 concentrations leaving NCA Bi radioisotopes in the aqueous phase. At 0.01 M 18-crown-6 concentration with 2 M HClO4, separation factor (S Tl/Bi) as high as 3.7 × 103 was achieved. The separation experiment was repeated with stable isotopes of Bi and Tl. The extent of separation was monitored by ICP-OES and the results corroborated with radiometric methods.

Advanced AIE Materials for Environmental Monitoring: Selective Sensing of Thorium(IV) in Aquatic Systems.

Thorium (Th) is commonly used in various applications, but its long-term exposure poses health risks, necessitating its detection in aqueous environments. Traditional methods such as inductively coupled plasma mass spectrometry are sensitive but require complex instrumentation. Optical sensors, particularly fluorometry-based methods, are simpler, cost-effective, and selective. However, developing effective aggregation-induced emission (AIE) turn-on sensors for Th(IV) requires water-soluble fluorophores with a low background fluorescence. In the present work, we report a turn-on detection method for Th(IV) based on the AIE of the fluorophore tetra(4-sulfophenyl) ethylene (SuTPE). Th(IV)-induced aggregation of SuTPE and the simultaneous drastic enhancement of the emission property of SuTPE have been utilized for the selective sensing of Th(IV) in 100% aqueous media. The sensing mechanism was explored using ground-state absorption, steady-state and time-resolved emission, FTIR, DLS, SEM, AFM and quantum chemical studies of the SuTPE-Th(IV) complex. The selectivity of the present probe toward Th(IV) ions has been established by studying the interference of several metal ions, including lanthanides and uranyl ions. The LOD for Th(IV) was estimated to be 240 nM (56 ppb). The performance of the probe was demonstrated in tap water and diluted seawater matrixes. This work provides a significant advance for Th(IV) detection in aqueous environments, with implications for environmental monitoring and health safety.

Fast and Sensitive Determination of Iodide Based on Ternary Chalcogenides Nanoparticles

A fluorescent probe based on ternary AgFeS2 quantum dots has been prepared for the design of ternary chalcogenides. The nanoparticles are synthesized with oleylamine as a stabilizer at a low temperature (particle size in the range of 2 to 3 nm) and they exhibit an intense blue emission in aqueous media. As for their internal structure, each nanoparticle’s relative stoichiometric ratio (AgFe1.01S1.91) is very close to the theoretical value of 1:1:2. Their magnetic properties have been studied with a vibrating sample magnetometer and they have ferromagnetism between 4 K and 298 K (applied magnetic field ranging between −10,000 and 10,000 Oe). In the presence of iodide ions, the emission at 458 nm derived from AgFeS2 QDs has been observed to give rise to fluorescence quenching. The detection system is based on a static quenching process and morphological change between iodide ions and AgFeS2, which has a good linear range from 0 to 37.5 μmol/L, with a limit of detection of 0.99 μM. The nanoprobe responds within 30 s for the efficient detection of iodide. Such functional quantum dots will provide a powerful indicator in environmental and bio-sensing applications.

Electrospun gelatin/tea polyphenol@pullulan nanofibers for fast-dissolving antibacterial and antioxidant applications.

Bio-based active food packaging materials have a high market demand. We use coaxial electrospinning technology to prepare core-shell structured nanofibers with sustained antibacterial and antioxidant properties. The fiber core layer was composed of gelatin and tea polyphenols, whereas tea polyphenols provide antibacterial and antioxidant properties; the fiber sheath was composed of pullulan polysaccharides with antioxidant properties. By using a scanning electron microscope, it can be seen that the diameter distribution of the prepared nanofibers was uniform and the surface is smooth; using a transmission electron microscope, it can be clearly seen that the nanofibers have a core-shell structure; Fourier Transform Infrared and X-ray diffraction analysis indicate that the nanofibers have an amorphous structure; the 2,2-diphenyl-1-picrylhydrazyl free radical scavenging shows that nanofibers have higher antioxidant properties with the addition of tea polyphenols; antibacterial test showed that nanofibers had obvious inhibitory effect on the growth of Staphylococcus aureus and Escherichia coli; and the nanofiber film dissolution test shows that nanofibers can be used as fast soluble active packaging. Finally, core-sheath-structured nanofibers can serve as active packaging for instant food, possessing both rapid water solubility and excellent antibacterial and antioxidant activity, making water-soluble nanofibers interesting applications in the field of food packaging.

A Water‐Soluble Cycloparaphenylene: Supramolecular Receptor with Visible Fluorescence

AbstractWe report the first synthesis of a water‐soluble [9]cycloparaphenylene derivative containing three hydrindacene (1,2,3,5,6,7‐hexahydro‐s‐indacene) units with four carboxylates at the 2,6‐positions via a macrocyclic gold complex. This crown‐shaped macrocyclic compound exhibits remarkable water solubility, of up to 16 mmol L−1 (2.6 g/100 mL), as well as strong visible fluorescence in water (λem=447 nm, ϕF=0.64, brightness (ϵ×ϕF)=5.1×104). This molecule effectively encapsulates cationic guest compounds, such as methyl viologen dichloride, as indicated by a change in visible fluorescence.

Progress in essential oil extraction and their applications in food packaging and preservation

AbstractEssential oils (EOs) are secondary metabolites synthesised by many aromatic plants, which have good antimicrobial and antioxidant activities making them popular functional agents for food preservation and packaging applications. In recent years, novel extraction techniques, such as super critical fluid extraction, pulsed electric field assisted extraction and ultrasound assisted extraction have been explored as alternatives to the conventional solvent‐based extraction methods. This review mainly discusses on recent progresses in sustainable extraction of essential oil (EO) from aromatic plants and food processing wastes and their functional properties, and applications in food preservation have also been summarised. Sustainable extraction techniques yield better‐quality EO due to low temperature and short time process compared to the conventional extraction. Despite efficacy of EOs as good active agents, their low water solubility, volatile nature, strong flavour, and susceptibility to food processing parameters are major challenges against their applications in food. These challenges can be mitigated by advanced techniques such as encapsulation and nanoemulsification of EO, which provide dual functions of enhanced applicability and improved functional properties. Incorporation of EO in the biopolymer‐based films and coatings can open avenues for sustainable food packaging and preservation.

Single-Step Extrusion Process for Formulation Development of Self-Emulsifying Granules for Oral Delivery of a BCS Class IV Drug.

This study aimed to develop and optimize formulations containinga BCS Class IV drug by improving its solubility and permeability. Herein development of self-emulsifying solid lipid matrices was investigated as carrier systems for a BCS Class IV model drug. Self-emulsifying drug delivery systems (SEDDS) have been extensively investigated for formulating drugs with poor water solubility. However, manufacturing SEDDS is challenging. These systems usually have low drug-loading capacities, and the incorporated drugs tend to recrystallize during storage, which severely impacts the storage stability in vitro and performance in vivo. Moreover, they require greater amounts (>80%) of lipid carriers, cosolvents, surfactants, and other excipients to keep them from recrystallizing. This in turn is again challenging for high-dose drugs as it affects the size of the final drug product (tablets and capsules). Also, the final liquid nature of the formulation affects the handling and processability of the formulation, which poses challenges during the manufacturing and packaging steps. In this work, we have studied the feasibility of a single-step extrusion process to formulate and optimize solid self-emulsifying granules with a relatively higher drug loading of Ritonavir (RTV), a BCS Class IV drug. Further, we have compared the performance of using these granules as the feedstock for direct powder extrusion-based 3D printing as opposed to the use of physical blends. The stability and solubility-permeability advantage of these granules was also evaluated where SEDDS showed about 27 and 20 fold increase in apparent solublity and permeability compared to bulk drug, respectively. Combining the capabilities of HME to form drug-loaded homogeneous granules as a continuous process along with application of direct printing extruiosn (DPE) 3D printing improves the drug delivery prospects for such candidates.

Synthesis of a novel water-soluble pyridine dicarboxylate and its application in fluorescence cell imaging

Abstract A novel water-soluble substituted pyridine dicarboxylate containing a quaternary ammonium ion with potential applications in fluorescence cell imaging was synthesized and characterized. Remarkably, this compound exhibited water solubility in the absence of additional solubilizers, enabling direct dissolution in phosphate-buffered saline for cell studies. No obvious cytotoxicity was observed in 4T1 cells (mouse breast cancer cells) within the concentration range of 0.2–25 μmol L−1, with a cell survival rate above 89%. Furthermore, the compound exhibited a maximum two-photon absorption cross-section of 86 GM at an excitation wavelength of 780 nm, demonstrating high cell permeability, effective distribution in the cytoplasm, and preferential targeting of organelles. Single- and two-photon fluorescence imaging of cells revealed a distinctive blue emission and strong bright green emission, respectively. The newly synthesized substituted pyridine dicarboxylate exhibited low cytotoxicity and strong fluorescence imaging properties, demonstrating its potential in cell imaging applications.

Investigations on the Impacts of Drugs or Excipients with Different Physicochemical and Compaction Properties on the Disintegration Behavior of Kollidon®SR-Based Binary Controlled Release Matrix Tablets.

The objective of this study was to examine the impact of the physicochemical properties of the loaded drug or excipient, the concentration of Kollidon®SR (KSR), and the mechanical characteristics of KSR compacts on their disintegration times. Using disintegration apparatus, a two-hour constraint was chosen as the process's end point. Lactose-KSR compacts subjected to the highest compression pressure and Microcrystalline cellulose-KSR compacts with KSR concentrations exceeding 30% exhibited disintegration times of less than ten minutes. Likewise, compacts containing Diltiazem HCl-KSR demonstrated brief disintegration times across all tested KSR concentrations and compression pressures. Compacts of Modafinil, Metformin HCl, and Ascorbic acid-KSR displayed disintegration times ranging from fast to moderate, contingent upon the levels of KSR and compression pressure applied. Compacts containing KSR with Aspirin, Salicylic acid, or Ibuprofen did not exhibit significant disintegration even at minimal amounts of KSR (0.5%). Theophylline-KSR tablets also showed prolonged dissolution times, even at very low concentrations of KSR. The disintegration times of Dic-KSR tablets were roughly close to an hour and were predominantly unaffected by varying KSR levels and only marginally influenced by compression pressures. It is possible to draw the conclusion that different drugs or excipients have different minimum KSR requirements to resist compacts' disintegration process. Compounds that demonstrate low solubility in water can result in extended disintegration times for KSR compacts. The melting points of these compounds, in conjunction with the Py values of the compacts and their compaction properties, could affect the disintegration process, although a precise evaluation is necessary.

Reduction of 2,4-dichlorophenoxy acetic acid herbicide toxicity from aqueous media by adsorption: Experimental and theoretical study using DFT method

This work studies the possibility of reducing the toxicity of water laden with 2,4-dichlorophenoxy acetic acid (2,4-D) using a commercial activated carbon (AC). Multiple structural and textural characterization techniques including Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM/EDS), point of zero charge (pHzpc) determination, Boehm titration, iodine number, Methylene blue index, and BET analysis measurements were performed on the commercial AC. Various parameters affecting adsorption were studied and well-known isotherms models in their linear and non-linear forms were applied for fitting equilibrium data. The kinetic data was analyzed using intraparticle diffusion, pseudo-first and second-order kinetic models. Density functional modeling (DFT) of 2,4-dichlorophenoxyacetic acid was used to investigate the origin of the reactivity. The AC surface area was found to be 1017 m2⋅g−1. A contact time of 30 min, an AC dose of 4 g⋅L−1 and a pH of 6.2 resulted in a maximum adsorption capacity of 235.55 ± 6.43 mg⋅g−1. The thermodynamic study revealed that the adsorption process was physical, spontaneous and endothermic. The adsorption process was governed by second-order kinetics and controlled by intraparticle diffusion.

Ultrafast surface esterification of cellulosic materials in aqueous media at room temperature

Ultrafast surface esterification of cellulosic materials in aqueous media at room temperature

Stability of hydrous basaltic melts at low water fugacity: evidence for widespread melting at the lithosphere-asthenosphere boundary

The upper mantle low velocity zone is often attributed to partial melting at the lithosphere-asthenosphere boundary. This implies that basaltic melts may be stable along plausible geotherms due to the freezing point depression in the presence of water and other incompatible impurities. However, the freezing point depression (ΔT) as a function of water content in the near-solidus basaltic melt (cH2O) cannot be precisely determined from peridotite melting experiments because of difficulties in recovering homogeneous basaltic glasses at high pressures. We therefore used an alternative approach to reinvestigate and accurately constrain the ΔT–cH2O relationship for basaltic melts at the low water fugacities that are expected in the upper mantle. Internally heated pressure vessel (IHPV) experiments were performed at water-saturated conditions in the anorthite-diopside-H2O system at confining pressures of 0.02 to 0.2 GPa and temperatures between 940 and 1450 ℃. We determined the water-saturated solidus, and obtained ΔT by combining our data with reports of dry melting temperatures in the anorthite-diopside system. In another series of experiments, we measured water solubility in haplobasaltic melts and extrapolated cH2O to pressures and temperatures of the water-saturated solidus. By combining the results from these two series of experiments, we showed that the effect of water on ΔT was previously underestimated by at least 50 ℃. The new ΔT–cH2O relationship was then used to revise predictions of melt distribution in the upper mantle. Hydrous melt is almost certainly stable beneath extensive regions of the oceanic lithosphere, and may be present in younger and water-enriched zones of the subcontinental mantle.

Solution and Surface Solvation of Nitrate Anions with Iron(III) and Aluminum(III) in Aqueous Environments: A Raman and Vibrational Sum Frequency Generation Study.

Hydrated trivalent metal nitrate salts, Fe(NO3)3·9H2O and Al(NO3)3·9H2O, in both solid and aqueous phases are investigated. Raman and surface-selective vibrational sum frequency generation (SFG) spectroscopy, are used to shed light on ion-ion interactions and hydration in several spectral regions spanning low frequency (440-550 cm-1) to higher frequency modes of nitrate and water (720, 1050, 1250-1450, and 2800-3750 cm-1). These frequencies span the metal-water mode, nitrate in-plane deformation, nitrate symmetric and asymmetric modes, and the OH stretch of condensed phase water molecules. Comparison to NaNO3, and in some cases KNO3, is also shown, providing insight. Splitting and frequency shifts are observed and discussed for both the solid state and solution phase. The Lewis acidity of Fe3+ and Al3+ ions plays a significant role in the observed spectra, in particular for the nitrate asymmetric band splitting and frequency shift. The spectral response from water solvation for iron and aluminum nitrates is nonlinear as compared to linear for sodium nitrate, suggesting significantly different solvation environments that are limited by water hydration capacity at higher concentrations. Moreover, a non-hydrogen bonded OH, dangling OH, from hydrating water molecules is observed spectroscopically for Al and Fe nitrate solutions. Furthermore, aluminum nitrate perturbs the surface water structure more than iron nitrate despite aluminum being a weaker Lewis acid. The surface water structure is thus found to be unique for the Al(NO3)3 solutions as compared to both Fe(NO3)3 and NaNO3, such that surface solvation is more pronounced. This observation exemplifies the nature of the Fe(III) and Al(III) ions and their substantial influence on the surface water structure.

Enhancing Environmental Remediation: Advancements in Chemically Crosslinked Cyclodextrin‐Based Materials for Organic and Inorganic Pollutant Removal

AbstractConcern over the harmful impacts of pollutants on human health and the environment has increased in recent decades due to their widespread presence in water resources. These pollutants include pesticides, poisonous textile dyes, and micropollutants. It is essential to remove these pollutants from wastewater to enhance the quality of water for industrial usage. Because of externally hydrophilic and internally hydrophobic qualities, cyclodextrin and its derivatives have shown great promise as adsorbents for the treatment of wastewater. While cyclodextrins cannot be used as adsorbents on their own due to their water solubility, they can be efficiently polymerized with different types of cross‐linkers to increase their stability and effectiveness. This review article examines chemically crosslinked materials based on cyclodextrin and its derivatives, utilizing various cross‐linkers such as epichlorohydrin, glutaraldehyde, citric acid, N,N′‐methylene bisacrylamide and maleic anhydride. These materials are evaluated for their effectiveness in adsorbing textile dyes, micropollutants, pharmaceuticals, and pesticides from wastewater. Additionally, this article provides a detailed explanation of adsorption kinetics, thermodynamics, and kinetic isotherms for the removal of contaminants. It also discusses the mechanism of contaminant adsorption, and reusability of adsorbents. Finally, this study delves into the challenges and exciting future prospects of CD‐based adsorbents, highlighting their potential to revolutionize wastewater treatment.