Extraction Procedure Research Articles

Routine method for the analysis of microplastics in natural and drinking water by pyrolysis coupled to gas chromatography-mass spectrometry

The presence of microplastics (MPs) in water intended for human consumption represents a growing concern due to their ubiquity in the aquatic environments and the potential adverse effects on human health. In this context, validated and standardized analytical methods are required to minimize uncertainties associated with the determination of MPs in water, especially during the drinking water treatment process. In this study, a simple water sampling and extraction procedure and analysis using pyrolysis with gas chromatography coupled to mass spectrometry (Py-GC-MS) was developed to determine 7 types of polymers in water. Quality parameters associated with the method were evaluated, including limits of detection (MDL) and quantitation (MQL), linearity, precision, accuracy, and extended uncertainty. The developed methodology was validated by participating in the EUROQCHARM interlaboratory exercise, and the Z-scores were within the acceptable range for 4 of the 5 polymers tested. Finally, MPs were determined in river water, reclaimed water, and drinking water from the urban area of Barcelona and total concentrations ranged from 11.3 µg/L to 77.1 µg/L. The proposed methodology allows for simple (direct filtration of 100-500 mL of water with a 13 mm glass fiber filter), quantitative (µg/L), and rapid (with a total analysis time of 20 minutes per sample, including both pyrolysis and GC-MS) analysis of MPs in water intended for drinking.

Electrochemical detection of atrial natriuretic peptide-coated nanocarriers based on a molecularly imprinted polymer receptor thin film

Molecular imprinting polymers (MIPs) are biomimetic materials of great interest in the scientific and industrial fields for the development of innovative sensing strategies. Herein, we proposed a new sensing application by developing an electrochemical sensor using molecular imprinting (MI) technology for recognition of atrial natriuretic peptide (ANP) both as a free molecule in solution and attached to nanoparticle-based drug delivery systems (DDSs), aiming to provide fast and reliable information on the cell uptake of nanoparticles (NPs). As proof of concept, poly(lactic-co-glycolic acid) (PLGA) NPs were synthesized and used as nanocarriers for ischemic heart disease therapy were synthesized and then functionalized with ANP (named here as PLGA-NPs@ANP). The MIP receptor film was prepared by electrochemical polymerization of dopamine over the working area of a gold screen-printed electrode (AuSPE), using cyclic voltammetry (CV) technique. The construction of the ANP sensor was carefully optimized to enhance its performance, including the film thickness and the procedures for effective template extraction from the MIP matrix. The MIP biosensor presented a linear response against polymeric NPs (PLGA-NPs@ANP) concentration logarithm ranging from 4.0 μg mL-1 to 100 μg mL-1, with a sensitivity of – 0.0129 mA mL μg-1 decade-1 and an LOD < 4.0 μg mL-1. Furthermore, the developed MIP receptor film was able to discriminate ANP-functionalized nanocarriers from non-functionalized NPs.

Effect of different oil extraction techniques for Moringa Peregrina seed on its meal content of glucosinolates

Background Moringa peregrina (M.P) is a multipurpose promising tree that grows widely in Asia and Africa’s tropical and subtropical regions. It is generally rich in nutrients especially oil which can be used for edible or nonedible purposes and also rich in protein. However, some anti-nutritional substances, namely glucosinolates (GSLs), remain in M.P meal preventing its utilization in animal or human feeding. These substances though good for the plant to defend against herbivores, cause deleterious effects or are even toxic to animals and humans. GSLs are the most important anti-nutritional substances in M.P seed and meal. Objective Accordingly, this investigation aims to use different techniques for oil extraction from M.P seed and their effect on the GSLs content of the meal remaining after oil extraction, then the meal is detoxified to be suitable for using in animal or human feeding. Materials and methods In this study, M.P meal was obtained as a by-product left over after oil extraction from moringa seed by different extraction procedures including (hydraulic press, screw pressing, extraction by solvent via Soxhlet, and prepress − solvent extraction at room temperature).The sinalbin, moringin, and total GSLs were determined and identified by HPLC. Detoxification of GSLs was then applied for M.P meal remaining after oil extraction by hexane, using soaking in water followed by a water-washing treatment. Results and conclusion The results indicated that sinalbin and moringin are the major dominant GSLs in M.P seed and meal. Moreover, the total GSLs content in the meal that remained after all different oil extraction techniques was significantly higher when compared with their content in the seed. Also, the results showed that there was a significant decrease in the level of total GSLs in M.P meal as a result of the water treatment. It decreased from 941.8±34.14 nmol/mg in defatted meal before water treatment to 23.97±18.31 nmol/mg in residues left after treatment with water for 15 min. Therefore, soaking in water followed by a water-washing treatment is the simplest and most efficient process to remove the GSLs from M.P meal to be suitable for animal feeding.

Demystifying the tropics: FTIR characterization of pantropical woods and their α-cellulose extracts for past atmospheric 14C reconstructions

To ensure unbiased tree-ring radiocarbon (14C) results, traditional pretreatments carefully isolate wood cellulose from extractives using organic solvents, among other chemicals. The addition of solvents is laborious, time-consuming, and can increase the risk of carbon contamination. Tropical woods show a high diversity in wood-anatomical and extractive composition, but the necessity of organic-solvent extraction for the 14C dating of these diverse woods remains untested. We applied a chemical treatment that excludes the solvent step on the wood of 8 tropical tree species sampled in South-America and Africa, with different wood-anatomical and extractive properties. We analyzed the success of the extractive removal along with several steps of the α-cellulose extraction procedure using Fourier Transform Infrared (FTIR) spectroscopy and further confirmed the quality of 14C measurements after extraction. The α-cellulose extracts obtained here showed FTIR-spectra free of signals from various extractives and the 14C results on these samples showed reliable results. The chemical method evaluated reduces the technical complexity required to prepare α-cellulose samples for 14C dating, and therefore can bolster global atmospheric 14C applications, especially in the tropics.

Integrated approach of ultrasound with mild heat treatment on the quality characteristics of yacon (Smallanthus sonchifolius) tuber juice

AbstractThe research delved into the ascendancy of thermosonication (TS) on elevating the alimentary components of yacon (Smallanthus sonchifolius) tuber juice, derived from the yacon plant. This investigation introduces an innovative approach utilizing artificial neural networks (ANNs) coupled with genetic algorithm (GA) for the multifaceted optimization of extraction procedures. It aims to pinpoint the most effective processing parameters for TS, including variations in amplitudes: X1 (40, 50, and 60%) and temperatures: X2 (30, 40, and 50°C) over sonication times: X3 (15, 30, 45, and 60 min). Further, the approach is focused to amplify quality of yacon juice (YJ) and microbial attributes by enhancing certain quality characteristics such as anti‐oxidant activity (AOA), ascorbic acid (AA), total phenolic content (TPC), total carotenoid content (TCC), total flavonoid content (TFC), yeast and mold count (YMC) and total viable count (TVC). The maximum levels of AOA (33.73 ± 2.21%), AA (25.82 ± 2.03 mg/100 ml), TPC (85.08 ± 3.67 mg GAE/ml), TCC (115.82 ± 2.46 βCE μg/ml), TFC (22.52 ± 2.11 mg QE/ml), TVC, and YMC (not detected) were achieved in thermosonicated YJs under optimal conditions using ANN coupled with GA.Practical ApplicationsYacon tuber juice (YJ) treated with thermosonication (TS) showed improved nutritional characteristics, making them a valuable source of functional compounds for nutraceuticals and food industries. Research emphasizes the effectiveness of artificial neural network in predicting the extraction efficiency of YJ and proposes TS as a potential replacement for traditional thermal pasteurization to maintain or enhance YJ quality and functionality. TS provides cost‐effective and sustainable solutions to the food industry by reducing processing time and energy consumption when compared to pasteurization.

Ethnic Differences, Lung Cancer Risk, and Association of NRF2 Gene Polymorphism with Gemcitabine-Based Chemotherapy.

The cancer burden is rising every year. Lung cancer is one of themost common cancers and non-small cell lung cancer is the most common type. Chemotherapy based on platinum drugs and third-generation nucleoside anti-metabolites such as gemcitabine are used widely. Gemcitabine has a complex metabolic pathway, with many mechanisms contributing to its cytotoxicity. Derangements in the metabolic pathway genes contribute to drug resistance and toxicity with this drug. Association studies including these genetic polymorphisms in the metabolic pathway, clinical outcomes, and cancer risk reported inter-individual differences. Thus, the aim of this study was to ascertain the role of these genetic variants in South Indian cancer patients treated with gemcitabine-based therapy. The study was done with 184 healthy volunteers for frequency establishment and 123 cancer patients were treated with gemcitabine-based chemotherapy for response and toxicity assessment. The participants were aged 18-65 years and resided in the southern states of India. DNA extraction was done from the leukocyte fraction of the blood by phenol-chloroform extraction procedures and genotyping was done by reverse transcription-polymerase chain reaction (RT-PCR) techniques to identify DNA repair gene polymorphisms. Tumor response was determined using Response evaluation criteria in solid tumors (RECIST) guidelines and toxicity using Common Terminology Criteria for Adverse Events (CTCAE), version 4.03. The patients were followed up for survival analysis. The minor allele frequency of the single nucleotide polymorphism (SNP) NRF2-617 C>A (rs6721961) in the healthy population was 12.8%. SNPs were in Hardy-Weinberg equilibrium (p>0.05). Gender-based differences were not observed with the studied SNP in the healthy population and the lung cancer patients. These frequencies of NRF2 were found to be similar when compared to EUR (European) and all the South Asian subpopulations. They are significantly divergent compared to AFR (African), AMR (American), and EAS (East Asian) populations. The minor allele frequency in cancer patients was found to be 14.2% and the lung cancer risk with the SNP studied could not be detected. There was no association found with the response, toxicity, and survival among lung cancer patients. NRF2, being a multifaced molecule, did not showa significant association with lung cancer risk, response, and toxicity in patients with gemcitabine-based chemotherapy.

Implementing magnetic molecularly imprinted solid phase extraction to analytical method for determination of 2-phenethylamine in cocoa powder and chocolate by LC-MS/MS system

The main aim of this study was to design, develop, and apply magnetic molecularly imprinted polymer (MMIP) during sample pretreatment before liquid chromatography tandem mass spectrometry (LC-MS/MS) 2-phenylethylamine determination in cocoa powder and chocolate samples. The morphology and structure of MMIP, obtained from methacrylic acid (monomer) and trimethylolpropane trimethacrylate (cross-linker) were characterized using scanning electron microscopy, nitrogen sorption analyses, infra-red spectroscopy, X-ray diffraction measurements, vibrating-sample magnetometry, and thermogravimetry analyses. The analyte adsorption mechanism on MMIP was studied using computational simulation. The magnetic solid phase extraction procedure on MMIP was optimized, resulting in a relative matrix effect of 6.2 % for cocoa powder and 2.8 % for chocolate. The LC-MS/MS quantified the 2-phenethylamine in eighteen cocoa powder and chocolate samples, showing a concentration range between 2.4 and 8.7 μg g−1.

AQbD-guided development and validation of an innovative extraction procedure and stability-indicating RP-HPLC method for quantification of posaconazole in tablet formulation

The objective of this work is to develop a stability-indicating HPLC method for the quantification of Posaconazole (PCZ) in tablet formulation using an Analytical Quality by Design (AQbD) approach. The development process involved the Design of Experiments (DOE) utilizing distinctive constraints mixture design for mobile phase ratio optimization and a 2-level factorial design for selection of extraction diluent compositions. Key responses measured included % assay and system suitability parameters. Method operable design regions (MODR) were determined, and final optimum conditions were selected. Forced degradation studies were conducted to assess method stability. The optimized HPLC method employed a Zorbax C18 column with a mobile phase consisting of pH 3.5 10mM phosphate buffer, acetonitrile, and methanol in a ratio of 30:53:17 % v/v/v. The method demonstrated stability-indicating capabilities, with PCZ degradation observed in acidic and oxidative environments, while remaining stable in alkali. Peak purity analysis from Empower software confirmed the absence of interaction with degradants. Validation according to ICH Q2 (R2) guidelines showed precision, linearity over the range of 0.25 µg/mL to 376 µg/mL, and accuracy demonstrated through recovery studies from 50 to 150%. The developed HPLC method utilizing AQbD approach is specific, robust, precise, and accurate for the quantification of PCZ in tablet formulations, thus suitable for routine analysis.

CH4 and CO2 adsorption–desorption-diffusion characteristics in surfactant-modified coal under microscopic conditions

Hydraulic techniques are integral to both coal mining and gas extraction procedures, and the precise inclusion of surfactants in hydraulic fracturing fluids serves as a crucial factor influencing the wettability of coal and facilitating gas desorption. Nevertheless, relatively few investigations have focused on the influence of surfactants within coal on the adsorption–desorption-diffusion dynamics of gases. In this study, Xin Tian high-rank coal was treated with different surfactants, and the pore structure and functional groups of the coal samples were determined by fluid invasion methods, Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and 13C nuclear magnetic resonance (13C NMR) spectroscopy. Moreover, molecular-scale models were constructed to simulate the adsorption–desorption-diffusion performance of the gases in the surfactant-modified coal. As per the results, modification with methyltrimethoxysilane (MTMS) and polyethylene oxide (PEO) surfactants reduced the proportion of micropores and relative content of oxygen functional groups, resulting in reduced the adsorption of gases and enhanced diffusion performance, consistent with molecular simulations result. These results provide a theoretical foundation for elucidating the adsorption–desorption mechanisms of surfactant-treated coal and its application in mining areas.

Comparison of Different Extraction and Purification Methods of Lime Peel Pectin and Evaluation of Physiochemical, Rheological, and Textural Properties

Background:: Pectin production has recently attracted considerable research interest due to its various applications arising from its unique characteristics. Lime peel, as a by-product of juice factories, has a promising potential for pectin extraction. Methods:: Lime peel pectin samples were extracted by three extraction processes: a) 90°C of heating for 120 min, b) 90°C of heating for 90 min and then 32 min of sonication, and c) 80°C of heating for 60 min and then 22 min of sonication. Then, they were purified either by ethanol or sodium caseinate (SC) and characterized. Results:: SC purification did not enhance the pectin yield; rather, it diminished the level of nonpectin components and resulted in purer pectin (i.e., lower sugar content). The samples purified with SC showed much lower viscosity in solution and storage modulus than the samples purified with ethanol, which could be attributed to their lower sugar content and higher pH (~ 4.6 vs. 2). However, pectin samples purified with SC had a relatively high sugar gel consistency, maybe due to protein retention in their structure as well as the preferential hydration effect of added sucrose. Conclusion:: The compact and extended conformations of the pectin sample, which was extracted by “(c) extraction method” and purified with ethanol, resulted in its high viscosity and storage modulus in solution and the highest gel consistency (16.91 Kg.s) compared to the other samples. Regardless of the conditions of extraction procedures, the purification method had a considerable impact on the pectin samples’ characteristics and potential applications.

A simulation approach for quantifying ballistic impact damage in ultra-high-performance concrete

In this work, we provide a hydrocode simulation model for high-velocity projectile impact against ultra-high-performance concrete targets and establish a methodology to extract damage quantities from the simulation results. In the parameter derivation process, published and own data stemming from material experiments, such as uniaxial, triaxial, and planar plate impact tests, are used as a starting point. To fill the systematic gaps of strength data for pressures of 1 GPa to 5 GPa and for fractured concretes, residual velocities of projectiles and qualitative target damage information from ballistic experiments with high-hard steel spheres are additionally used as a reference in parametric simulations. All criteria from the comparatively broad data basis are successfully reproduced by the simulation model simultaneously. The simulated damage quantities derived by the proposed extraction procedure are reasonable counterparts to the corresponding experimental measures from earlier published works, allowing a new quality of comparison between both worlds.

Integration of miniaturized sample preparation and molecularly imprinted polymers in food analysis

The use of innumerable chemical compounds in food production to enhance agricultural quality and yield has raised significant global concerns regarding food safety. To address these concerns, miniaturized solid sample preparation techniques have emerged as an appealing strategy for analyzing chemical residues in complex samples, notably those found in food matrices. The efficacy of these miniaturized solid extraction procedures hinges largely on the choice of the sorbent phase. Molecularly imprinted polymers (MIPs) have been introduced as highly selective and versatile sorbent phases for a wide range of miniaturized solid techniques. Their remarkable selectivity is attributed to the creation of distinct cavities during the synthesis process, which subsequently accommodate the target analyte when the sample is applied. This unique characteristic empowers MIP polymers to exhibit exceptional specificity toward the desired analyte. The use of MIPs as sorbent phases in miniaturized sample preparation methods has shown great potential to increase the analytical performance of residue evaluation in food matrices. Therefore, here we present a comprehensive overview of the current landscape of miniaturized solid sample techniques employing MIPs as sorbent phases for the assessment of residues in food samples. Moreover, this review is primarily on recent reports concerning the application of MIPs in solid-phase microextraction (SPME), in-tube SPME, microextraction by packed sorbent (MEPS), disposable pipette extraction (DPX), solid-phase extraction in pipette tip (SPE-PT) and stir bar sorptive extraction (SBSE). Lastly, we will bring some future topics concerning the use of MIPs in miniaturized sample preparation methods for food analysis in order to bring some new avenues for enhancing food products' safety and quality assessment.

Data Mining Techniques Against Cyber Threats: A Review

Abstract Data mining is a technique used to extract useful data from existing databases. Those datasets are now being shared globally. Secure communication and confidentiality are required because data from multiple sources must be collected and stored in one central location. Data mining technology involves methods that rapidly and efficiently convert vast quantities of data into relevant insights adapted to the user's requirements. Unfortunately, the utilization of data mining expertise to acquire sensitive personal information poses a threat to individuals' privacy rights. This paper provides a review of the current techniques for preventing cyber risks and safeguarding privacy through the application of data mining. Data mining is used to examine, analyze, and figure out the structure and behavior of data mining organizations. Implementing data mining with optimal outcomes is a challenging task. In the past decade, academics have extensively studied many elements of data extraction. Therefore, it is crucial to provide published research evidence pertaining to this field. For this study, a thorough evaluation was carried out of more than thirty research papers sourced from reputable literature databases. The objective was to extract significant information regarding the field of data mining. The collected data was then used to address various study inquiries about cutting-edge extraction methodologies, data mining mechanisms in cyber dangers, data extraction procedures, algorithms, and evaluation techniques. This paper discusses various research areas and issues in data mining, serving as a valuable reference for researchers in this domain.

Optimizing anomaly detection in 3D MRI scans: The role of ConvLSTM in medical image analysis

The analysis of Medical Images (MI), particularly the detection and classification of anomalies in 3D MRI (Magnetic Resonance Imaging) scans, plays a critical part in timely intervention and personalized therapy plans. In our paper, a comprehensive methodology for anomaly detection in 3D MRI scans of the brain is proposed that combines advanced Deep Learning (DL) techniques, including Convolutional Long Short-Term Memory (ConvLSTM) model, with efficient statistical feature extraction from segmented anomaly regions. The data collection phase utilizes three main datasets namely the Brain Tumor Segmentation Challenge (BRATS), the Federated Tumor Segmentation Challenge (FETS), and the Medical Segmentation Decathlon (MSD). The research begins with preprocessing steps including image resizing, intensity normalization, and alignment of anomaly region segmentation masks. The targeted anomaly regions within the samples are segmented using U-Net architecture and then follow statistical feature extraction procedure. Dimensionality reduction methods such as Principal Component Analysis (PCA) and Recursive Feature Elimination (RFE) are utilized to streamline the feature space. The ConvLSTM is then used to classify the anomalies using both convolution and recurrent layers to capture spatiotemporal patterns in MRI data. The model is fine-tuned and iterated for better classification performance using Adam optimizer. The statistical evaluation results with accuracy of 98.9 % showed that the designed ConvLSTM method is more suitable for clinical diagnosis and treatment design in detecting anomalies in 3D MRI images.

Ineffective Strategies in Scientific Communication: Textual Wordiness vs. Clarity of Thought in Thesis Conclusion Section

Introduction. The issue of lexical redundancy in academic writing remains crucial. Research based on Russian-language corpora is vital for the development of effective targeted academic writing courses that meet the unique needs of universities. This paper aims to identify factors through examples of wordiness in the Conclusion sections of theses to alter the design of courses broadening academic writing skills to fight against textual redundancy at various educational levels. Materials and Methods. A corpus of 72 theses across three educational levels (Bachelor’s, Master’s, and Candidate degrees) was analyzed. We selected theses from the repositories of the HSE University and Moscow City University. We focused on Conclusion section due to its highest level of conciseness: textual redundancy critically impacts its effectiveness. The analysis included a comprehensive procedure of raw data extraction, coding, conceptualization during iterative discussions, and classification according to Brohaugh’s taxonomy. Results. “Invisible” type of wordiness is a prevalent issue in academic writing across all levels of education. Such types as “overkill”, “weak-kneed” and “empty” occur more frequently in research in Master’s and Candidate’s theses. The need to comprehend the reasons behind the use of different types of wordiness and their impact on readability is stressed. Candidate’s theses are wordier despite the expectation of a higher level of academic writing skills at this level. Discussion and Conclusion. The study highlights the systemic role of academic writing courses at all educational levels in reducing text wordiness. Despite our expectations of advanced writing skills in Candidate’s theses, their high level of wordiness indicates the need for developing effective academic writing strategies. It is crucial to implement a personalized approach to academic writing instruction, considering the specific needs and challenges of each educational level, to create more concise academic texts. The paper provides insights into approaches to designing academic writing courses.

Unveiling New Arsenic Compounds in Plants via Tailored 2D-RP-HPLC Separation with ICP and ESI MS Detection.

Arsenic (As) speciation analysis is scientifically relevant due to the pivotal role the As chemical form plays in toxicity, which, in turn, directly influences the effect it has on the environment. The objective of this study was to develop and optimize a method tailored for studying As compounds in plant samples. Different extraction procedures and HPLC methods were explored to assess their efficiency, determine mass balance, and improve the resolution of compounds in the chromatograms. Conventionally applied anion-exchange chromatography facilitated the separation of well-documented As compounds in the extracts corresponding to 19 to 82% of As present in extracts. To gain insight into compounds which remain undetectable by anion chromatography (18 to 81% of As in the extracts), but still possibly metabolically relevant, we explored an alternative chromatographic approach. The procedure of sample purification and preconcentration through solid-phase extraction, facilitating the detection of those minor As compounds, was developed. The system was further refined to achieve an online 2D-RP-HPLC system, which was employed to analyze the extracts more comprehensively with ICP and ESI MS. Using this newly developed method, As(III)-phytochelatins, along with other arseno-thio-compounds, were detected and identified in extracts derived from the tree roots of seedlings grown in the presence of As(III) and As(V), and a group of arseno lipids was detected in the roots of plants exposed to As(V).

Stability of Propolis Phenolics during Ultrasound-Assisted Extraction Procedures.

Propolis has gained popularity in recent years as a potential preventive and therapeutic agent due to its numerous health benefits, which include immune system boosting, blood pressure lowering, allergy treatment, and skin disease treatment. The pharmacological activity of propolis is primarily attributed to phenolics and their interactions with other compounds. Given that phenols account for most of propolis's biological activity, various extraction methods are being developed. The resin-wax composition of the propolis matrix necessitates the development of an extraction procedure capable of breaking matrix-phenol bonds while maintaining phenol stability. Therefore, the aim of this study was to assess the stability of two major groups of phenolic compounds, flavonoids and phenolic acids, in propolis methanol/water 50/50 (v/v) extracts obtained after ultrasound-assisted extraction (USE) under different extraction parameters (extraction time and pH) and heat reflux extraction (HRE). The methodology involved varying the USE parameters, including extraction time (5, 10, and 15 min) and pH (2 and 7), followed by analysis using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to quantify phenolic recoveries. Results revealed that benzoic acid and chlorogenic acid derivatives demonstrated excellent stability across all ultrasound extraction procedures. The recoveries of flavonoids were highly diverse, with luteolin, quercitrin, and hesperetin being the most stable. Overall, neutral pH improved flavonoid recovery, whereas phenolic acids remained more stable at pH = 2. The most important optimization parameter was USE time, and it was discovered that 15 min of ultrasound resulted in the best recoveries for most of the phenols tested, implying that phenols bind strongly to the propolis matrix and require ultrasound to break the bond. However, the high variability in phenol extraction and recovery after spiking the propolis sample shows that no single extraction method can produce the highest yield of all phenols tested. As a result, when working with a complex matrix like propolis, the extraction techniques and procedures for each phenol need to be optimized.

Bio-analytical Methodology for Exploring Ripretinib’s Pharmacokinetic Profile in Rat Plasma Employing Bosutinib as an Internal Standard Utilizing LC-MS/MS

A robust, consistent, straightforward, swift, and precise liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was tailored for the bioanalytical analysis of ripretinib, with bosutinib serving as the comparative standard. This article provides a synopsis of recent developments in bioanalytical LC-MS/MS techniques utilizing a phenyl column (150x4.6 mm, 3.5 μ) and an eluting agent composed of ammonium formate at a pH of 2.5, which was altered in a 50:50 ratio with formic acid and acetonitrile. The chromatogram was utilized to analyse ripretinib, and the MS detector was equipped with electrospray ionization (ESI) method functioning in positive ionization conditions with multiple reactions monitoring (MRM). This allowed for the recording of transition m/z values of 531.4465→170.9638 for ripretinib and 511.4230 → 160.7133 for BTB. In the chromatographic analysis, ripretinib was retained for approximately 2.433 minutes, whereas BTB was retained for around 3.608 minutes. The validity of the approach extends across a linearity scale of 5 to 100 ng/mL for ripretinib, boasting a correlation index of 0.9999. In the realm of biological matrices, the extraction procedure employing the protein precipitation technique yields recovery rates of 99.6, 99.2, and 98% at the lower, middle, and higher quality control levels, respectively. The obtained results for accuracy, precision, matrix effect, and stability were determined to be within the acceptable range. To observe the investigated analyte in bodily fluids, pharmacokinetic studies yielded key parameters, including a half-life of 10 hours and a time to reach a maximum drug level of 4 hours. This thorough assessment affirms that the method satisfies rigorous criteria for system suitability and specificity well within predefined acceptance limits. Such performance positions it as an indispensable asset in the realm of bioanalysis, significantly broadening its clinical applicability.

Bio-analytical Methodology for Exploring Ripretinib’s Pharmacokinetic Profile in Rat Plasma Employing Bosutinib as an Internal Standard Utilizing LC-MS/MS

A robust, consistent, straightforward, swift, and precise liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was tailored for the bioanalytical analysis of ripretinib, with bosutinib serving as the comparative standard. This article provides a synopsis of recent developments in bioanalytical LC-MS/MS techniques utilizing a phenyl column (150x4.6 mm, 3.5 μ) and an eluting agent composed of ammonium formate at a pH of 2.5, which was altered in a 50:50 ratio with formic acid and acetonitrile. The chromatogram was utilized to analyse ripretinib, and the MS detector was equipped with electrospray ionization (ESI) method functioning in positive ionization conditions with multiple reactions monitoring (MRM). This allowed for the recording of transition m/z values of 531.4465→170.9638 for ripretinib and 511.4230 → 160.7133 for BTB. In the chromatographic analysis, ripretinib was retained for approximately 2.433 minutes, whereas BTB was retained for around 3.608 minutes. The validity of the approach extends across a linearity scale of 5 to 100 ng/mL for ripretinib, boasting a correlation index of 0.9999. In the realm of biological matrices, the extraction procedure employing the protein precipitation technique yields recovery rates of 99.6, 99.2, and 98% at the lower, middle, and higher quality control levels, respectively. The obtained results for accuracy, precision, matrix effect, and stability were determined to be within the acceptable range. To observe the investigated analyte in bodily fluids, pharmacokinetic studies yielded key parameters, including a half-life of 10 hours and a time to reach a maximum drug level of 4 hours. This thorough assessment affirms that the method satisfies rigorous criteria for system suitability and specificity well within predefined acceptance limits. Such performance positions it as an indispensable asset in the realm of bioanalysis, significantly broadening its clinical applicability.

Biotic regulation of phoD-encoding gene bacteria on organic phosphorus mineralization in lacustrine sediments with distinct trophic levels

Organic phosphorus (Po) mineralization hydrolyzed by alkaline phosphatase (APase) can replenish bioavailable P load in the sediment water ecosystem of lakes. However, the understanding about the interaction between P load and bacteria community encoding APase generation in the sediment are still limited. Different P pools in the sediments from Taihu Lake, China were measured using sequential extraction procedure. The APAase activity (APA) were obtained accompanying with enzymatic dynamical parameters Vmax and Km. The abundances and diversity of gene phoD-harboring bacterial communities were assessed using high throughput sequencing. The analysis results showed the decrease of potentially bioavailable P fractions including MgCl2-P and Fe-P along sampling gradient southwards together with active P concentrations in the water. Conversely, increasing APA and absolute abundance of phoD gene were found with the decreasing of P loads southwards. Positive correlation (p<0.05) between absolute abundance and APA indicated that phoD-encoding bacteria manipulated the APA and Po mineralization. Negative correlation (p<0.01) suggested that the APA was restrained by high P load and was promoted under low P condition. However, higher Vmax and Km values suggested that high mineralization potential of Po maintained the high concentrations of potentially bioavailable P even the APA was restricted. The abundance increase of predominant genus Cobetia (from 15.51 to 24.34 %) mirrored by the reduced Calothrix abundance (from 24.65 to 1036 %) was speculated to be responsible for the APA promotion under low P condition. Higher diversity indices in the high P scenario suggested that high P load stimulated the ecological diversity of gene phoD-encoding bacteria community. Generally, rare taxa such as Burkholderia having high connected degrees in bacterial communities together with abundant genera synergistically manipulated the phoD gene abundance and APase generation. Interaction between P fractions and bacteria encoding phoD gene determined the eutrophication status in the lacustrine ecosystem.