Preparation Method Research Articles

Intact quantitation of cysteine-conjugated antibody-drug conjugates using native mass spectrometry.

A common strategy for antibody-drug conjugate (ADC) quantitation from in vivo study samples involves measurement of total antibody, conjugated ADC, and free payload concentrations using multiple reaction monitoring (MRM) mass spectrometry. This not only provides a limited picture of biotransformation but can also involve lengthy method development. Quantitation of ADCs directly at the intact protein level in native conditions using high-resolution mass spectrometers presents the advantage of measuring exposure readout as well as monitoring the change in average drug-to-antibody ratio (DAR) and in vivo stability of new linker payloads with minimal method development. Furthermore, site-specific cysteine-conjugated ADCs often rely on non-covalent association to retain their quaternary structure, which highlights the unique capabilities of native mass spectrometry (nMS) for intact ADC quantitation. We developed an intact quantitation workflow involving three stages: automated affinity purification, nMS analysis, and data processing in batch fashion. The sample preparation method was modified to include only volatile ion-pairing reagents in the buffer systems. A capillary size-exclusion chromatography (SEC) column was coupled to a quadrupole time-of-flight high-resolution mass spectrometer for high-throughput nMS analysis. Samples from two mouse pharmacokinetic (PK) studies were analyzed using both intact quantitation workflow and the conventional MRM-based approach. A linear dynamic range of 5-100 μg/mL was achieved using 20 μL of serum sample volume. The results of mouse in vivo PK measurement using the intact quantitation workflow and the MRM-based approach were compared, revealing excellent method agreement. We demonstrated the feasibility of utilizing nMS for the quantitation of ADCs at the intact protein level in preclinical PK studies. Our results indicate that this intact quantitation workflow can serve as an alternative generic method for high-throughput analysis, enabling an in-depth understanding of ADC stability and safety in vivo.

One-step spray solution combustion synthesis of nanostructured spherical Ca3Co4O9: The fuel effect

In the research, a one-step method for the rapid preparation of spherical nanostructured particles of Ca3Co4O9, involving the combustion of reactive aerosol drops containing calcium and cobalt nitrates as the metal precursors and hexamethylenetetramine as the fuel, is reported. The results of thermodynamic analysis and study of crystalline structure of obtained materials suggest that the reaction in the investigated system proceeds with heat release, which indicates its self-sustaining nature. Applying hexamethylenetetramine fuel at φ range of 0.4 – 0.6 and ambient temperature of 900 ℃ resulted in formation of Ca3Co4O9 powders with narrow particle size distribution of 0.2 – 1 µm. Microstructural studies revealed that the Ca3Co4O9 particles are hollow with nanometer-scale wall thicknesses and their surface consists of lamellar grains with sizes ranging from 14 to 100 nm.

Application of N-doped NiCo2O4 / NiO / Co3O4 composites rich in oxygen vacancies in electromagnetic wave absorption.

In this work, N-doped and oxygen vacancy-rich NiCo2O4/NiO/Co3O4 composites are synthesized by the direct calcination method. Noticeably, by changing the additive concentrations of urea dissolved in DMF (N-N dimethylformamide), the electromagnetic (EM) wave absorption abilities of NiCo2O4/NiO/Co3O4 composite effectively. A maximum reflection loss (RLmax) value at 12.94 GHz for a 2.8 mm thick sheet is -29.76 dB, while its effective absorption bandwidth (EAB) (RL<-10 dB) reaches 4.21 GHz. In-depth research of possible mechanisms of EM wave absorption enhancement. Owing to its simple preparation method and superb EM wave absorption properties, the NiCo2O4/NiO/Co3O4 composites have a chance to be suitable candidates for high-property EM wave absorbers.

Polypyrrole Derivatives: Preparation, Properties and Application

Polypyrrole (PPy) has attracted widespread attention due to its excellent environmental stability, high conductivity, simple synthesis, good biocompatibility, and reversible redox properties. PPy derivatives not only inherit the advantages of polypyrrole, but also have some unique properties. The side and N-site substitution of PPy can not only yield polymers with good solubility, but it also endows polymers with special functionalities by controlling the introduced functional groups. The performance of copolymers can also be adjusted by the type of monomer or polymerization ratio. In this review, an overview of the different types, main preparation methods, and the application prospects of PPy derivatives reported to date are summarized and presented. The current challenges and future opportunities in this research area are also prospected.

Chitosan/Silica Hybrid Nanogels by Inverse Nanoemulsion for Encapsulating Hydrophilic Substances

AbstractA strategy for the preparation of a hybrid chitosan/silica nanohydrogel is reported, which combines the gelation of chitosan in a nanoemulsion system with a sol–gel process to produce silica. Chitosan is used as a biopolymer matrix, while silica acts as a structuring additive. Hydrogel nanocapsules are obtained through the ionic interaction of the cationic groups of chitosan with the anionic groups of sodium triphosphate (STP), which is used as a physical cross‐linker. Two alternative preparation methods are compared in this work: in the first one, STP is added to the continuous phase of an inverse emulsion of chitosan; in the second one, the fusion of droplets of two emulsions containing separate chitosan and STP takes place. The size of the obtained nanocapsules ranges from 50 to 200 nm. The efficiency of the formed hydrogel for entrapping a hydrophilic model substance (erioglaucine disodium salt) is investigated for the two systems by studying the release in a neutral aqueous medium. The results indicate that the hydrophilic cargo is efficiently encapsulated by both preparation methods, although the droplet‐fusion method yields more stable suspensions. As a general observation, the release behavior of erioglaucine is systematically retarded when silica is present in the systems.

Deoxygenative Geminal Silylboration of Amides Using Silylboronates: Synthesis and Use of α-Boryl-α-Silylalkylamines.

α-Silylalkylamines and α-borylalkylamines are versatile synthetic intermediates and attractive scaffolds found in pharmaceutical drugs and agrochemicals. Despite great progress on synthetic methods for preparation of α-silylalkylamines or α-borylalkylamines, there are no general strategies for preparation of α-boryl-α-silylalkylamines and the reactivity has not been explored. Here we report deoxygenative geminal silylboration of amides using silylboronates in the presence of alkoxide base catalyst, producing α-boryl-α-silylalkylamines. The silicon and boron groups in α-boryl-α-silylalkylamines are found to be utilized to chemoselective transformations, such as protonation and alkylation. This protocol serves various α-silylalkylamines and α-borylalkylamines from readily available amides.

Deoxygenative Geminal Silylboration of Amides Using Silylboronates: Synthesis and Use of α‐Boryl‐α‐Silylalkylamines

α‐Silylalkylamines and α‐borylalkylamines are versatile synthetic intermediates and attractive scaffolds found in pharmaceutical drugs and agrochemicals. Despite great progress on synthetic methods for preparation of α‐silylalkylamines or α‐borylalkylamines, there are no general strategies for preparation of α‐boryl‐α‐silylalkylamines and the reactivity has not been explored. Here we report deoxygenative geminal silylboration of amides using silylboronates in the presence of alkoxide base catalyst, producing α‐boryl‐α‐silylalkylamines. The silicon and boron groups in α‐boryl‐α‐silylalkylamines are found to be utilized to chemoselective transformations, such as protonation and alkylation. This protocol serves various α‐silylalkylamines and α‐borylalkylamines from readily available amides.

Colloidal Templating in Catalyst Design for Thermocatalysis.

Conventional catalyst preparative methods commonly entail the impregnation, precipitation, and/or immobilization of nanoparticles on their supports. While convenient, such methods do not readily afford the ability to control collective ensemble-like nanoparticle properties, such as nanoparticle proximity, placement, and compartmentalization. In this Perspective, we illustrate how incorporating colloidal templating into catalyst design for thermocatalysis confers synthetic advantages to facilitate new catalytic investigations and augment catalytic performance, focusing on three colloid-templated catalyst structures: 3D macroporous structures, hierarchical macro-mesoporous structures, and discrete hollow nanoreactors. We outline how colloidal templating decouples the nanoparticle and support formation steps to devise modular catalyst platforms that can be flexibly tuned at different length scales. Of particular interest is the raspberry colloid templating (RCT) method which confers high thermomechanical stability by partially embedding nanoparticles within its support, while retaining high levels of reactant accessibility. We illustrate how the high modularity of the RCT approach allows one to independently control collective nanoparticle properties, such as nanoparticle proximity and localization, without concomitant changes to other catalytic descriptors that would otherwise confound analyses of their catalytic performance. We next discuss how colloidal templating can be employed to achieve spatially disparate active site functionalization while directing reactant transport within the catalyst structure to enhance selectivity in multistep catalytic cascades. Throughout this Perspective, we highlight developments in advanced characterization that interrogate transport phenomena and/or derive new insights into these catalyst structures. Finally, we offer our outlook on the future roles, applications, and challenges of colloidal templating in catalyst design for thermocatalysis.

Systematic Review of Platelet-Rich Plasma in Medical and Surgical Specialties: Quality, Evaluation, Evidence, and Enforcement

Background: Platelet-rich plasma (PRP) is widely used in various medical and surgical specialties for its regenerative properties, including aesthetics (facial rejuvenation, hair restoration, and skin tightening) and orthopedics (treatment of tendinitis and osteoarthritis). However, the inconsistent literature on PRP’s efficacy and safety leads to critical knowledge gaps. This systematic review evaluates quality control measures in PRP preparation and application and explores the regulatory environment governing its clinical use. Methods: Following PRISMA guidelines, a comprehensive search was conducted across multiple databases, including PubMed, EMBASE, and Web of Science, for studies published from January 2020 to April 2024. The review included randomized controlled trials (RCTs) involving human participants undergoing PRP treatment for aesthetic or regenerative purposes. Key parameters such as the PRP preparation methods, platelet concentration, and quality control measures were analyzed. The study protocol was registered with PROSPERO (ID: CRD42024557669). Results: Out of 75 RCTs involving 5726 patients, the review identified significant variability in PRP preparation methods and application techniques, including differences in centrifugation protocols and platelet concentration levels. A new evidence-based scoring system, the William–Eqram Scoring System for PRP Quality Reporting (WESS-PQR), was proposed to address these inconsistencies. Correlation analysis revealed a strong positive correlation (r = 0.79) between proper temperature control during preparation and PRP efficacy. Initial platelet count assessment showed a moderate positive correlation (r = 0.57) with efficacy. Conclusions: Standardized PRP preparation protocols and robust regulatory frameworks are urgently needed to ensure the safety and efficacy of PRP treatments. The proposed WESS-PQR scoring system can serve as a valuable tool for clinicians and researchers, promoting consistency and reliability in PRP applications.

Grain Manipulation by Annealing Treatment Realizes High-Performance N-Type Bi2Te2.4Se0.6 Thermoelectric Material and Device.

Bi2Te3-based materials play a crucial role in solid cooling and power generation, but the rapidly deteriorated ZT with rising temperatures above 450 K severely limits further applications. Here, this paper reports a novel preparation method of annealing treatment for molten ingot, which can enhance the thermoelectric performance of n-type Bi2Te2.4Se0.6 in a wide temperature range. Instead of conventional halides, copper is adopted to regulate the carrier concentration and grain size to optimal levels. During the process of annealing at 573 K for 4h, the number of twins significantly increases and the grains of Cu-doped samples become larger and more oriented. These optimizations lead to higher carrier mobility with similar carrier concentration compared with the sample without heat treatment. The synergistic effects of Cu doping and annealing treatment realize a high average ZT of 0.89 within 300-600 K in n-type Cu0.02Bi2Te2.4Se0.6. Combined with p-type (Bi,Sb)2Te3, the fabricated thermoelectric device exhibits a high conversion efficiency of 6.9% at a temperature difference of 300 K. This study suggests that annealing treatment is a simple and effective scheme to promote the applications of n-type Bi2(Te,Se)3 in a wide temperature range.

Quantitative Comparison of Deparaffinization, Rehydration, and Extraction Methods for FFPE Tissue Proteomics and Phosphoproteomics.

Formalin-fixed paraffin-embedded (FFPE) tissues are suitable for proteomic and phosphoproteomic biomarker studies by data-independent acquisition mass spectrometry. The choice of the sample preparation method influences the number, intensity, and reproducibility of identifications. By comparing four deparaffinization and rehydration methods, including heptane, histolene, SubX, and xylene, we found that heptane and methanol produced the lowest coefficients of variation (CVs). Using this, five extraction methods from the literature were modified and evaluated for their performance using kidney, leg muscle, lung, and testicular rat organs. All methods performed well, except for SP3 due to insufficient tissue lysis. Heat n' Beat was the fastest and most reproducible method with the highest digestion efficiency and lowest CVs. S-Trap produced the highest peptide yield, while TFE produced the best phosphopeptide enrichment efficiency. The quantitation of FFPE-derived peptides remains an ongoing challenge with bias in UV and fluorescence assays across methods, most notably in SPEED. Functional enrichment analysis demonstrated that each method favored extracting some gene ontology cellular components over others including chromosome, cytoplasmic, cytoskeleton, endoplasmic reticulum, membrane, mitochondrion, and nucleoplasm protein groups. The outcome is a set of recommendations for choosing the most appropriate method for different settings.

Ce–Zr–Mn Oxide Catalysts for Soot Combustion: The Role of Preparation Method

Ce–Zr–Mn Oxide Catalysts for Soot Combustion: The Role of Preparation Method

Design and application of an ultrasensitive and selective tobromycin electrochemiluminescence aptasensor using MXene /Ni/Sm-LDH-based nanocomposite.

Using a chemiluminescence reaction between luminol and H2O2 in basic solution, an ultrasensitive electrochemiluminescence (ECL) aptasensor was developed for the determination oftobramycin (TOB), as an aminoglycoside antibiotic. Ti3C2/Ni/Sm-LDH-based nanocomposite effectively catalyzes the oxidation of luminol and decomposition of H2O2, leading to the formation of different reactive oxygen species (ROSs), thus amplifying the ECL signal intensity of luminol, which can be used for the determination of TOB concentration. To evaluate the performance of the electrochemiluminescence aptasensor and synthesized nanocomposite, different methods such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) analyses were performed. The considerable specific area, large number of active sites, and enhanced electron transfer reaction on this nanocomposite led to the development of an ECL aptasensor with high sensitivity and electrocatalytic activity. After optimizing the preparation method and analysis conditions, the aptasensor revealed a wide linear response ranging from 1.0 pM to 1.0 μM with a detection limit of 18 pM, displaying outstanding accuracy, specificity, and response stability. The developed ECL sensor was found to be applicable to the determination of TOB in human serum samples and is anticipated to possess excellent clinical potentials for detecting other antibiotics, as well.

Amorphous Solid Dispersions: Implication of Method of Preparation and Physicochemical Properties of API and Excipients

The present study investigated the effect of different polymers and manufacturing methods (hot melt extrusion, HME, and spray drying, SD) on the solid state, stability and pharmaceutical performance of amorphous solid dispersions. In the present manuscript, a combination of different binary amorphous solid dispersions containing 20% and 30% of drug loadings were prepared using SD and HME. The developed solid-state properties of the dispersions were evaluated using small- and wide-angle X-ray scattering (WAXS) and modulated differential scanning calorimetry (mDSC). The molecular interaction between the active pharmaceutical ingredients (APIs) and polymers were investigated via infrared (IR) and Raman spectroscopy. The in vitro release profile of the solid dispersions was also evaluated to compare the rate and extend of drug dissolution as a function of method of preparation. Thereafter, the effect of accelerated stability conditions on the physicochemical properties of the solid dispersions were also evaluated. The results demonstrated higher stability of Soluplus® (SOL) polymer-based solid dispersions as compared to hydroxypropyl methylcellulose (HPMC)-based solid dispersions. Moreover, the stability of the solid dispersions was found to be higher in the case of API having high glass transition temperature (Tg) and demonstrated higher interaction with the polymeric groups. Interestingly, the stability of the melt-extruded dispersions was found to be slightly higher as compared to the SD formulations. However, the down-processing of melt-extruded strands plays critical role in inducing the API crystal nuclei formation. In summary, the findings strongly indicate that the particulate properties significantly influence the performance of the product.

Preparation and properties of especially pure Ge-Sb-As-S glasses for IR optics

The novel multi-stage method for preparation of especially pure GexAsySbzS100-x-y-z (x = 10–13; y = 20–23; z = 4–6) glasses is presented. The method includes the stages of deep purification of initial elements using different chemical getters, transport reactions and vacuum distillation. The glass samples with compositions close to stoichiometric ones and a low content of gas-forming impurities are synthesized; their structure, optical, thermal and magneto-optical properties are investigated. The studied characteristics of the samples meet the requirements for their use in the IR optics and are relevant for multifunctional applications.

In-situ immobilization of ZIF-67/ZIF-8 on wood biomass for degradation of methylene blue and formaldehyde

Metal-organic frameworks (MOFs) have been extensively studied for the removal of pollutants in wastewater and air. However, the existence of MOF materials in powder form with easy agglomeration and difficult separation has greatly confined their application potential. To address this challenge, ZIF-67/ZIF-8 composites were in-situ grown on wood biomass, with its porous structure providing channels for the growth of MOFs and active sites for MOFs catalysis. The structure, i.e., morphology, crystallinity and chemical components, and optical properties were characterized. The degradation efficiency of methylene blue (MB) by the ZIF-67/ZIF-8@wood composites photocatalyst was more than 85.7 % under visible light irradiation within 90 mins, reflecting the good photocatalytic activity of the composites. The ZIF-67/ZIF-8@wood composites completely adsorbed and decomposed HCHO (22.3 ppm) within 30 mins. The high catalytic performance of the ZIF-67/ZIF-8@wood composites can be attributed to the high surface area of wood that results in a high absorption of contaminants. This simple, low-cost, and green preparation method has promoted the sustainable utilization of biomass resources with great significance for practical environmental remediation.

Microencapsulation: A Review

A process known as "microencapsulation" forms thin wall material coverings around things, which can be gases, liquids, or even solids, and encases them in tiny particles. Small entities with an active ingredient known as the core material encased in a covering substance or embedded in a matrix structure are known as microencapsulated products, or micro particles. The overview includes information on encapsulating materials, preparation methods, the physics of release through the capsule wall, microcapsule characterization, and the many applications of microcapsules. The review, "State of Art of Microencapsulation of Microcapsule Preparation Process Technology," is a reputable resource on the creation, characteristics, and applications of novel small particles that are individually encapsulated. It also covers popular microencapsulation techniques and their benefits and drawbacks, as well as the broader applications of these techniques in the fields of pharmaceuticals, cosmetics, agriculture, food technologies, and textiles.

Fe-doped TiO2/PVDF-HFP electrospun membranes for tetracycline photocatalytic degradation under visible light

Heterogeneous photocatalysis operated under visible light is considered an efficient and ecofriendly method to remove pharmaceuticals from water streams. However, the recovery of the nano-sized catalyst particles limits this technology to small-scale applications. In this study, we prepared Fe-doped P25 TiO2 photocatalysts and immobilized them over PVDF-HFP electrospun membranes for the photocatalytic degradation of Tetracycline antibiotic under visible light. To ensure uniform distribution of the nanoparticles on the fibers, the electrospinning voltage and the weight percentage of TiO2 were varied, and two preparation methods were applied to disperse the catalyst in the polymeric solution. In order to maximize the visible light exposure of the membranes, 3D printed membrane holders with square and circular shapes were designed to immerse the membrane in Tetracycline solution. The results showed that immobilizing P25 catalysts on the fibers of the membranes limited their visible light absorption when the light source was assembled on the top of the aqueous reaction medium. This occurred due to the membrane's opacity limited light penetration, resulting in uneven irradiation throughout its depth. Based on this, a new photocatalytic reactor design was proposed with immersed light illumination source to reduce the distance between the membrane and the light source for improved activation of the P25 particles. In this design, a 3D-printed vertical membrane holder was also included to accommodate a larger membrane surface area and therefore minimize the required spatial area for large industrial applications.

Encapsulating Fe3O4 Nanoparticles and Carbon Dots in a Metal-Organic Framework for Magnetic Fluorescent Taggants.

Magnetic fluorescent composite nanomaterials have broad application prospects in the fields of biological imaging, anticounterfeiting identification, suspicious object tracking, and identification of latent fingerprints in forensic medicine. For an effective taggant, a clearly visible identifying mark is necessary to enable observers to capture labeling information quickly and accurately, even from a distance. The preparation method of magnetic fluorescent composite materials is complicated and usually needs different surface modification and assembly processes. The limited loading capacity of fluorescent materials also limits the fluorescence properties of the composite, so it is difficult to produce obvious fluorescence as a taggant to meet the requirements of visible labeling. In this study, a core-shell structure of a magnetic fluorescent composite was prepared by using the metal-organic framework ZIF-8 as the host of fluorescent materials and an encapsulation shell coated on the Fe3O4 nanoparticles. The porous ZIF-8 is beneficial for increasing the loading capacity of fluorescent materials to ensure the fluorescence performance of the composite materials. Further modification of the composite surface prevented the desorption of fluorescent materials from the pores of ZIF-8, enabling the samples to maintain good fluorescence properties even after multiple washing cycles. The preparation method is simple, rapid, and cost-effective, and the prepared magnetic fluorescent composite nanomaterial has high magnetic separation performance and fluorescence performance, making it a promising material for identification, marking, and tracking.

Matrix effects in ultra-high performance supercritical fluid chromatography-mass spectrometry analysis of Vitamin E in plasma: the effect of sample preparation and data processing

The approaches to matrix effects determination and reduction in ultra-high performance supercritical fluid chromatography with mass spectrometry detection have been evaluated in this study using different sample preparation methods and investigation of different calibration models. Five sample preparation methods, including protein precipitation, liquid-liquid extraction, supported liquid extraction, and solid phase extraction based on both “bind and elute” and “interference removal” modes, were optimized with an emphasis on the matrix effects and recovery of 8 forms of vitamin E, including α-, β-, γ-, and δ- tocopherols and tocotrienols, from plasma. The matrix effect evaluation included the use and comparison of external and internal calibration using three models, i.e., least square with no transformation and no weighting (1/x0), with 1/x2 weighting, and with logarithmic transformation. The calibration model with logarithmic transformation provided the lowest %-errors and the best fits. Moreover, the type of the calibration model significantly affected not only the fit of the data but also the matrix effects when evaluating them based on the comparison of calibration curve slopes. Indeed, based on the used calibration model, the matrix effects calculated from calibration slopes ranged from +92% to – 72% for α-tocopherol and from -77% to +19% in the case of δ-tocotrienol. Thus, it was crucial to calculate the matrix effect by Matuszewski's post-extraction approach at six concentration levels, as a strong concentration dependence was observed for all optimized sample preparation methods, even if the stable isotopically labelled internal standard (SIL-IS) was used for the compensation. The significant differences between individual concentration levels and compounds were observed, even if the tested calibration range covered only one order of magnitude. In methods with wider calibration ranges, the inappropriate use of calibration slope comparison instead of the post-extraction addition approach could result in false negative results of matrix effects. For the selected example of vitamin E, solid-phase extraction was least affected by matrix effects when used in interference removal mode, but supported liquid extraction resulted in the highest recoveries. We showed that the calibration model, the use of a SIL-IS, and the analyte concentration level played a crucial role in the matrix effects. Moreover, the matrix effects can significantly differ for compounds with similar physicochemical properties and close retention times. Thus, in all bioanalytical applications, where different analytes are typically determined in one analytical run, it is necessary to carefully select the data processing in addition to the method for the sample preparation, SIL-IS, and chromatography.