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The widespread application of enzymes in industrial chemical synthesis requires efficient process control to maintain high yields and purity. Flow injection analysis-electrospray ionization-mass spectrometry (FIA-ESI–MS) offers a promising solution for real-time monitoring of these enzymatic processes, particularly when handling challenging compounds like sugars and glycans, which are difficult to quickly analyze using liquid chromatography-mass spectrometry due to their physical properties or the requirement for a derivatization step beforehand. This study compares the performance of FIA-MS with traditional hydrophilic interaction liquid chromatography (HILIC)-ultra high-performance liquid chromatography (UHPLC)-mass spectrometry (MS) setups for the monitoring of the enzymatic synthesis of N-acetyllactosamine (LacNAc) using beta-1,4-galactosyltransferase. Our results show that FIA-MS, without prior chromatographic separation or derivatization, can quickly generate accurate mass spectrometric data within minutes, contrasting with the lengthy separations required by LC–MS methods. The rapid data acquisition of FIA-MS enables effective real-time monitoring and adjustment of the enzymatic reactions. Furthermore, by eliminating the derivatization step, this method offers the possibility of being directly coupled to a continuously operated reactor, thus providing a rapid on-line methodology for glycan synthesis as well. [ABSTRACT FROM AUTHOR]

The objective of this study was to compare the plasma (PL) and seminal plasma (SP) pharmacokinetic profile of ceftiofur (CEFT) and desuroylceftiofur acetamide (DFCA) after administration of CEFT crystalline-free acid (CCFA) by SC route in two sites of the ear in beef bulls. Four clinically healthy Hereford bulls received a comprehensive physical exam and subsequently a breeding-soundness examination, CBC, and chemistry profile panel. All bulls were diagnosed healthy and satisfactory potential breeders. In one group (n = 2), a single dose of CCFA was administered SC route at the base of the ear (BOE) at a dose of 6.6 mg/kg of body weight. The second group (n = 2) was also administered by SC route in the middle third of the posterior aspect of the ear (MTE). The concentrations of CEFT and DFCA in PL and SP were determined by a high-performance liquid chromatography mass spectrometry (HPLC-MS). Blood and semen samples were collected before the administration of CCFA and at 12, 24, 36, 48, 72, 96, 120, 144, and 168 h after injection. No levels of CEFT were detected in PL and only in 20 of the 40 SP samples (P = 0.0001). The mean level of CEFT in SP was 0.11 % in comparison with the DFCA level. DFCA was found in all PL and SP samples. Therefore, DFCA was chosen to be utilized in the study of the pharmacokinetics parameters both in PL and SP. There were no differences in the mean PL levels of DFCA for the two sites of SC administration between the BOE (102.9 ± 78.9 ng/mL; X ± SD) and to MTE (116.1 ± 70.2 ng/mL; P = 0.58). The mean SP levels of DFCA after administration in the BOE was 857 ± 747 ng/mL, and for the MTE was 549 ± 488 ng/mL without differences between both sites (P = 0.15). The mean level of DFCA in PL was 109.5 ± 74.0 ng/mL, which was lower than the mean SP levels of 695 ± 103 ng/mL (P = 0.001). Moreover, the PL peak DFCA concentration (C max) was 229 ± 46 ng/mL at 36.0 ± 29.4 h (T max) post-administration. The SP C max was 1851 ± 533 ng/mL at 30.0 ± 28.6 h (T max) post-administration. The C max between PL and SP were distinctive (P = 0.004) without any differences in T max between PL and SP (P = 0.60). The terminal half-life for PL DFCA (47.4 ± 29.3 h) was not different than in SP (53.1 ± 23.6 h; P = 0.77). The PL area under the curve concentration time from the first to the last sample (AUC 0–last) was 18,984 ± 4841 ng/mL/h, which was significatively smaller compared with 125,677 ± 59,445 ng/mL/h for SP AUC 0–last (P = 0.04). The PL mean residence time from the first to the last sample (MRT 0–last) was 69.7 ± 15.1 h, and it was similar than for SP of 66.5 ± 7.7 h (P = 0.69). From the present investigation, based in its pharmacokinetic features, it was concluded that CCFA should be an appropriate antibiotic that could be used for the treatment of bull genital infections when its indication is properly outlined. To study the pharmacokinetics of CCFA in SP, DFCA metabolite was appropriated. [ABSTRACT FROM AUTHOR]

Microplastics (MPs) in the air are one of the major concerns due to their possible health risks. In addition, airborne microplastics act as a carrier for several toxic air pollutants and cause carcinogenic, mutagenic and teratogenic effects. Nylon 66 is one of the most abundant MPs in the microenvironments. In this study, we report an optimized method for the quantification of nylon 66 MPs present in the fine particulate matter (PM2.5) using high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The optimized method exhibited excellent linearity, recovery rates, intraday and interday precision and sensitivity. The optimized method was deployed to carry out a pilot study to measure the mass concentrations of nylon 66 microplastics present in the inhalable fraction of particulate matter collected in a shopping complex. The observed mass concentrations of nylon 66 MPs in this study are in the range from 0.30 ng m−3 to 4.37 ng m−3. This study demonstrates the presence of inhalable fraction of nylon 66 MPs in the indoor environment and their mass concentrations were determined using HPLC-MS/MS. [ABSTRACT FROM AUTHOR]

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AbstractMineral weathering played a critical role in removing highly concentrated carbon dioxide (CO2) from the Precambrian atmosphere. Currently, it plays an important role in biogeochemical cycles and soil formation in terrestrial ecosystems. We aimed to fix CO2 by crystallizing carbonated minerals obtained from weathered rocks into calcium carbonate (CaCO3). In this study, we isolated a new Enterobacter bacteria (UT18) species from soil containing many rocks and plants by comparing the ability of the isolated bacteria to decrease pH. In combination with the results of high-performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS), we demonstrated that UT18 participates in mineral weathering by secreting gluconic acid and acetic acid. These organic acids can release Ca, Al, and Si from anorthite. Traces of weathering on the anorthite surface were observed using scanning electron microscopy (SEM). The released Ca ions can be recrystallized by the addition of Na2CO3 into the formation of CaCO3 in the form of aragonite. Our study describes a new characteristic of acid production in UT18 and demonstrates an example of an H+-releasing pattern in microbial mineral weathering. This study will help elucidate the mechanism of microbial mineral weathering and can be applied to soil improvement and greenhouse effect mitigation. [ABSTRACT FROM AUTHOR]

Currently, phylloremediation has emerged as a highly effective method for eliminating air pollutants, particularly polyaromatic hydrocarbons (PAHs). When PAHs accumulate on the phyllosphere, they significantly impact the fungal communities residing on leaf surfaces. This study aimed to investigate how pollution distribution patterns affect the diversity and PAH-degrading abilities of phyllosphere fungi, alongside identifying suitable mathematical models for PAH degradation. Leaf samples from two locations, Maradana and Sapugaskanda, were identified as having the highest PAH concentrations through principal component analysis. The fungal diversity in these highly contaminated regions was varied, with dominant species exhibiting greater PAH-degrading capabilities than those in less polluted areas. Thirty-five morphologically different epiphytic fungal strains were isolated on Potato Dextrose Agar (PDA) medium using the sample leaf wash. Two different fungal strains were selected as the best PAH degraders among those 35 different strains. These fungal strains were identified as Trichoderma harzianum P4M-16, and Fusarium solani P11M-46 based on ITS sequence data. Notably, these fungal species were more prevalent in highly polluted urban areas compared to less contaminated sites. High-Performance Liquid Chromatography (HPLC) analysis revealed that these two fungal species degrade PAHs more efficiently than others. Their kinetics assays demonstrated alignment with four degradation models when breaking down phenanthrene, naphthalene, pyrene, and anthracene. Scanning electron microscopy images showed that these fungi function as endophytes, extending their mycelium into the core leaf tissue layers beyond the epidermis. Gas Chromatography-Mass Spectrometry (GCMS) analysis indicated that F. solani P11M-46 produced non-toxic byproducts during the breakdown of phenanthrene and anthracene, confirming their eco-friendly nature. Overall, our findings suggest the promising potential of using phyllosphere fungi in bioremediation processes for environmental pollutants such as PAHs. [ABSTRACT FROM AUTHOR]

Background: Pralsetinib, a targeted inhibitor of the RET enzyme, plays a critical role in the treatment of adult patients with locally advanced or metastatic non-small cell lung cancer (NSCLC) characterized by RET gene fusion mutations following platinum-based chemotherapy. Nevertheless, impurities resulting from the manufacturing and degradation of pralsetinib have the potential to impact its therapeutic effectiveness and safety profile. Methods: To address this issue, a liquid chromatography method was developed and validated for the specific identification of pralsetinib and its related impurities. The separation of pralsetinib and its related impurities was achieved via a Waters X Bridge Ci8 column with dimensions of 4.6 mm x 250 mm and a particle size of 5 ^m. Mobile phase A was composed of 20 mmol/L potassium dihydrogen phosphate (KH2PO4) and acetonitrile (ACN) at a volume ratio of 19:1, while mobile phase B consisted solely of ACN, utilizing a gradient elution technique. Detection was performed at a wavelength of 260 nm, with an injection volume of 10 ^L and a flow rate of 1.0 mL/min. Results: The chromatographic method established in this study was validated according to the ICH Q2 (R1) guidelines. The method demonstrated excellent linearity over a specific concentration range (imp-A: 0.035-10.21 ^ig/mL; imp-B: 0.09-10.16 ^g/mL; imp-C: 0.15-10.19 μg/mL; pralsetinib: 0.04-10.32 ^g/mL). Additionally, the method possesses high sensitivity, with detection limits for impurities A, B, C, and pralsetinib of 0.01, 0.03, 0.015, and 0.013 ^g/mL, respectively, and quantification limits of 0.035, 0.09, 0.05, and 0.04 ^ig/mL, respectively. In terms of specificity, stability, repeatability, accuracy, and robustness, the method met the validation acceptance criteria. Overall, the chromatographic technique established in this study can effectively separate pralsetinib and its impurities, providing reliable assurance for the accurate detection and quantification of impurities. Conclusion: The chromatographic method developed in this study can be utilized for the detection of pralsetinib and its impurities, offering a crucial reference for research on the quality of pralsetinib. [ABSTRACT FROM AUTHOR]

AbstractMethiocarb is a carbamate pesticide and is widely used due to its short lifetime but is a health concern due to its toxicity. To address this challenge, a novel nano-sorbent (zinc aluminate hybrid doped onto a magnetic activated carbon cloth (magnetic ACC@ZnAl2O4)) was synthesized. The characterization of the composite was done using FTIR spectroscopy, SEM, XRD, and EDX. The synthesized composite was then employed for the efficient extraction of methiocarb from food samples. Under the optimum conditions of (pH: 7.0, vortex time: 0.5 min, adsorbent dose: 5 mg, initial volume of sample: 50 mL, volume of eluent: 1.0 mL), quantitative recovery values of methiocarb in food samples were obtained (80–114%). This method impresses with its exceptional sensitivity, achieving incredibly low detection (LOD: 20 µg L−1) and quantification (LOQ: 67 µg L−1) limits for methiocarb. Its efficiency is equally impressive, with high values of preconcentration factor (PF: 50) and enhancement factor (EF: 49.4), ensuring accurate and reliable analysis with a low value of relative standard deviation (RSD: 4.8%). The method’s impressive selectivity, evident in its minimal interference from other pesticides, paves the way for reliable methiocarb analysis in food samples. [ABSTRACT FROM AUTHOR]

Quantifying the degree of deterioration is crucial for developing prevention strategies for archaeological leather. In this work, the morphology, chemical compositions, and physical properties of artificially aged leather samples were analyzed using a series of test methods to determine non-destructive or micro-destructive technologies for quantifying the degree of deterioration in archaeological leather. Results show that the hydroxyproline (Hyp) content of leather decreases with the increase of deterioration degree because deterioration leads to the gradual destruction of the collagen fiber network of leather. Moreover, the Hyp content of leather can be micro-destructively determined by high-performance liquid chromatography with fluorescence detection. Therefore, the determination of Hyp content is recommended to quantify the degree of deterioration in archaeological leather. [ABSTRACT FROM AUTHOR]

AbstractHb Youngstown [HBB:c.305A > C] is a rare unstable hemoglobin caused by the substitution of glutamic acid with alanine at codon 101 of the Beta globin chain. It causes hemolytic anemia in the heterozygous state. This is a case of a six-year-old Chinese-Javanese girl with heterozygous Hb Youngstown and clinical features of chronic hemolysis and iron overload. Hb Youngstown appears at the S window near to 4.6 minutes on high-performance liquid chromatography (HPLC) and can form a hybrid tetramer on alkaline gel electrophoresis seen as two distinct bands cathodal to A and close to F. For the first time, Hb Youngstown is captured with capillary electrophoresis (CE) and shown to be eluted at zone 8. Clinical presentation and Hb analysis results of this heterozygous Hb Youngstown overlap with heterozygous Hb Rush. They can only be differentiated at molecular level by Beta globin gene sequencing or intact mass spectrometry. [ABSTRACT FROM AUTHOR]

This article presents an efficient one-step synthesis of tetrahydropyrazolo[1,5- a ]pyrimidines through the recyclization of N -arylitaconimides with aminopyrazoles. The heterocyclic system of pyrazolo[3,4- b ]pyrimidine is known for its diverse biological properties, making its derivatives significant in pharmaceutical and medicinal chemistry. The study focuses on the regio- and chemoselective cascade reaction of N -arylitaconimides with 5-aminopyrazoles, demonstrating a new approach to synthesizing pyrazolo[1,5- a ]pyrimidines and pyrazolo[3,4- b ]pyridines. The methodology, involving boiling in isopropyl alcohol with acetic acid, yields selectively either pyrazolo[3,4- b ]pyridines or pyrazolo[1,5- a ]pyrimidines based on the substituents in the aminopyrazoles. The study elucidates the reaction mechanism, structural characterization using NMR spectroscopy, and confirms the structures via high-performance liquid chromatography and mass spectrometry. The simplicity and synthetic potential of this approach make it a valuable method for the preparation of these heterocyclic frameworks. [ABSTRACT FROM AUTHOR]

Voriconazole is a broad-spectrum triazole antifungal agent. A number of studies have revealed that the impact of C-reactive protein (CRP) on voriconazole pharmacokinetics was associated with the CYP2C19 phenotype. However, the combined effects of CYP2C19 genetic polymorphisms and inflammation on voriconazole pharmacokinetics have not been considered in previous population pharmacokinetic (PPK) studies, especially in the Chinese population. This study aimed to analyze the impact of inflammation on the pharmacokinetics of voriconazole in patients with different CYP2C19 genotypes and optimize the dosage of administration. Data were obtained retrospectively from adult patients aged ≥16 years who received voriconazole for invasive fungal infections from October 2020 to June 2023. Plasma voriconazole levels were measured via high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). CYP2C19 genotyping was performed using the fluorescence in situ hybridization method. A PPK model was developed using the nonlinear mixed-effect model (NONMEM). The final model was validated using bootstrap, visual predictive check (VPC), and normalized prediction distribution error (NPDE). The Monte Carlo simulation was applied to evaluate and optimize the dosing regimens. A total of 232 voriconazole steady-state trough concentrations from 167 patients were included. A one-compartment model with first order and elimination adequately described the data. The typical clearance (CL) and the volume of distribution (V) of voriconazole were 3.83 L/h and 134 L, respectively. The bioavailability was 96.5%. Covariate analysis indicated that the CL of voriconazole was substantially influenced by age, albumin, gender, CRP, and CYP2C19 genetic variations. The V of voriconazole was significantly associated with body weight. An increase in the CRP concentration significantly decreased voriconazole CL in patients with the CYP2C19 normal metabolizer (NM) and intermediate metabolizer (IM), but it had no significant effect on patients with the CYP2C19 poor metabolizer (PM). The Monte Carlo simulation based on CRP levels indicated that patients with high CRP concentrations required a decreased dose to attain the therapeutic trough concentration and avoid adverse drug reactions in NM and IM patients. These results indicate that CRP affects the pharmacokinetics of voriconazole and is associated with the CYP2C19 phenotype. Clinicians dosing voriconazole should consider the patient’s CRP level, especially in CYP2C19 NMs and IMs. [ABSTRACT FROM AUTHOR]

Introduction: Epididymal lumen fluids provides a stable microenvironment for sperm maturation. Ca2+ binding protein CABS1 is known to maintain structural integrity of mouse sperm flagella during epididymal transit of sperm. Besides, CABS1 was reported to contain anti-inflammatory peptide sequences and be present in both human saliva and plasma. However, little is known about the role of CABS1 in regulation of the microenvironment of epididymal lumen fluids.Methods: To further confirm the role of CABS1 in epididymis, we identified the expression of CABS1 in epididymal lumen fluids. Moreover, high performance liquid chromatography, coupled with tandem mass spectrometry technique was used to analyze the metabolic profiles and in vivo microperfusion of the cauda epididymis and inductively coupled plasma mass spectrometry (ICP-MS) assays was used to detect the concentration of metal ion of mouse cauda epididymal lumen fluids in CABS1 deficient and normal mice.Results: The results showed that CABS1 is present in epididymal lumen fluids, and the concentration of calcium in epididymal lumen fluids is not changed in Cabs1-/- male mice. Among 34 differential metabolites identified in cauda epididymis, 21 were significantly upregulated while 13 were significantly downregulated in KO cauda epididymis. Pathway analysis identified pyrimidine metabolism, inositol phosphate metabolism, arachidonic acid metabolism, purine metabolism and histidine metabolism as relevant pathways in cauda epididymis.Discussion: The perturbations of mitochondrial dysfunction and inflammation may be the crucial reason for the poor performance of Cabs1-/- sperm. [ABSTRACT FROM AUTHOR]

Background: Hypertension is a prevalent health condition with severe implications for cardiovascular health. Combination therapy involving Candesartan and Nifedipine has emerged as a promising approach for managing hypertension due to the synergistic effects of these medications. Methods: This study aimed to develop a Design of Experiment (DoE) based Green High-Performance Liquid Chromatography (HPLC) method for the simultaneous estimation of Candesartan and Nifedipine in a combined dosage form. Reversed-phase HPLC was utilized with UV-Vis spectrophotometry for detection. DoE principles were applied to optimize chromatographic conditions, including pH, ethanol percentage in the mobile phase, and flow rate. Results: Optimal chromatographic separation was achieved using a composite mobile phase comprising ethanol and potassium dihydrogen phosphate buffer (45:55, v/v) at pH 3.7, with a flow rate of 1 mL/min. Statistical analysis confirmed the significance of these parameters in achieving efficient separation. The developed method exhibited high precision, accuracy, and reliability across various validation parameters, including specificity, linearity, repeatability, and robustness. Conclusion: The proposed DoE-based Green HPLC method offers a sustainable and efficient approach for the simultaneous estimation of Candesartan and Nifedipine in hypertension management. By integrating green chemistry principles with systematic method development, this method provides a reliable analytical tool for routine quality control purposes in pharmaceutical formulations containing these medications. [ABSTRACT FROM AUTHOR]

Background: Diabetes Mellitus Type II (DM-II) and periodontitis are interlinked chronic conditions with complex pathophysiological mechanisms. Micronutrient deficiencies have been implicated in both conditions, but the evaluation of their serum profile in individuals with DM-II and periodontitis remains underexplored. Understanding the micronutrient status in these populations could provide valuable insights into their nutritional needs and potential therapeutic interventions. Materials and Methods: Serum samples were collected from DM-II patients with periodontitis (n=50), healthy individuals with periodontitis (n=50), and healthy controls without periodontitis (n=50). Micronutrient analysis was performed using high-performance liquid chromatography (HPLC) to quantify levels of vitamins (e.g., A, C, D, E), minerals (e.g., zinc, iron, magnesium), and antioxidants (e.g., selenium, glutathione). Statistical analysis was conducted using ANOVA and post-hoc tests to compare micronutrient levels among the groups. Results: In DM-II patients with periodontitis, serum levels of vitamin C were significantly lower (p < 0.05) compared to both healthy individuals with periodontitis and healthy controls without periodontitis. Similarly, levels of vitamin D and zinc were significantly decreased (p < 0.05) in DM-II patients with periodontitis compared to healthy controls without periodontitis. However, no significant differences were observed in the levels of other micronutrients among the groups. Conclusion: This study highlights distinct alterations in the serum micronutrient profile of DM-II patients with periodontitis, particularly lower levels of vitamin C, D, and zinc. These findings suggest the importance of nutritional interventions targeting these deficiencies in managing the comorbidity of DMII and periodontitis. Further research is warranted to elucidate the mechanistic links between micronutrient status and the pathogenesis of these chronic conditions. [ABSTRACT FROM AUTHOR]

Nine actinobacterial isolates were purified from the sediment sample of Kogilvai village, Warangal, Telangana, based on their capability to grow on the minimal medium with Ferulic acid (FA) as only Carbon (C) source. FA to Vanillin conversion capacity of these isolates was identified by Thin-layer chromatography (TLC). Biotransformation of FA to Vanillin was high by four isolates, S1, S3, O3 and O4 when compared to other five isolates (O1, O2, S2, S4 and S5) with initial pH 7 in basal medium. Among these four isolates, optimal and rapid FA to Vanillin bioconversion of 140 mg/L was shown by isolate S1 with UV-spectrophotometry. Its conversion was confirmed by High Performance Liquid Chromatography (HPLC) analysis with retention time of 2.9 min after 28hrs of incubation at 37°C with 1g/L ferulic acid in the medium with 150 rpm. Isolate S1 could utilize Lactose, Maltose, Glycerol, Fructose, Galactose, Sucrose, Dextrose, L-Arabinose, ONPG, Esculin and not other carbohydrates present in the Himedia Hicarbo kit. Molecular characterization showed that 16S rDNA gene sequence of isolate S1 was 98.27% similar to Limosilactobacillus fermentum CECT 562 with completeness of 96.7% and was identified as Limosilactobacillus sp. 16S rDNA gene sequence of isolate S1 was submitted to NCBI GenBank and its accession number was OR136396. As this isolate has high potential of FA to Vanillin biotransformation capacity, it can be further explored to be used for industrial setups for commercial exploitation. [ABSTRACT FROM AUTHOR]

Background Hemoglobin (Hb) Hekinan II (A27; Glu-Asp) is an α-chain variant, and its interaction with the common Southeast Asian (--SEA/) α-thalassemia (α-thal) deletion is rarely reported. This study provides a clinical update of Hb Hekinan II associated with (--SEA/) α-thal. Methods A total of 11 simple heterozygotes and 20 composite heterozygotes for Hb Hekinan II and (--SEA/) α-thal were included based on molecular diagnosis. Results Hb Hekinan II exhibited a significant increase in hemoglobin, mean corpuscular volume, and mean corpuscular hemoglobin content, but a decrease in red blood cell level compared with α+ thalassemia deletion. Compared with (--SEA/) α-thal, composite heterozygotes for Hb Hekinan II and (--SEA/) α-thal showed similar erythrocyte parameters. Both heterozygotes with and without (--SEA/) α-thal showed low Hb A2 level. Hb Hekinan II showed abnormal performance in high-performance liquid chromatography but not in capillary electrophoresis. Conclusion Hb Hekinan II is a benign Hb variant. The heterozygotes exhibit clinically asymptomatic coinheritance with (--SEA/) α-thal having comparable hematological phenotype to simple (--SEA/) α-thal. The combination of hematological and molecular analysis helped to improve the detection rate of this rare variant. [ABSTRACT FROM AUTHOR]

Objectives Voxelotor can increase hemoglobin levels in patients living with sickle cell disease (SCD). A clinician who is monitoring voxelotor response may want to know whole-blood voxelotor concentration, but this cannot be measured in most clinical settings. However, voxelotor has been demonstrated to cause "peak splitting" in common methods of hemoglobin measurement such as capillary zone electrophoresis (CZE) and high-performance liquid chromatography (HPLC). We hypothesized that we could use the size of the peak split to estimate the whole-blood concentration. Methods Blood from people with SCD was dosed with known concentrations of voxelotor, and multiparameter regression was used to derive the relationship of voxelotor concentration to the degree of peak splitting observed. To validate these equations, 21 patients started on voxelotor at 1500 mg/d had blood samples drawn at days 0, 14, 30, and 60. Samples were sent out for gold standard voxelotor concentration testing. The derived equations were then used to calculate voxelotor concentration. Results Calculated concentrations correlated strongly with measured concentrations for both CZE (R 2 = 0.83, P <.001) and HPLC (R 2 = 0.76, P <.001). Voxelotor concentration also had a significant effect on increases in hemoglobin (R 2 = 0.40, P <.001). Conclusions Thus, peak splitting CZE and HPLC can be used to estimate voxelotor concentration. [ABSTRACT FROM AUTHOR]

The separation of silybin A (SilA) and B (SilB) diastereomers in optically pure compounds is challenging due to their very similar physical and chemical properties. However, such separation is crucial for evaluating the biological activity of the diasteroisomers SilA and SilB, which show very different performance in pharmacological applications like treating prostate cancer, liver diseases, and Alzheimer's disease. The most common isolation method is based on high-performance liquid chromatography, but it is slow and has a yield in pure SilB of hundreds of milligrams per day. An alternative chemo-enzymatic separation method, utilizing an immobilized lipase CALB catalyst to stereoselectively acetylate silybin B (1b), offers advantages in terms of higher productivity, selectivity, and scalability, particularly when applied in flow reactors. This study delves into the kinetics of Sil acetylation catalyzed by Novozym 435 in a continuous flow milli-reactor, investigated at various temperatures, volumetric flow rates, and Sil initial concentrations. It is noteworthy that, at the current state of the art, there is a lack of kinetic studies on this reaction, emphasizing the novelty and significance of this work. The kinetic and fluid dynamic parameters were estimated using a non-linear regression analysis of experimental data. The examined reaction showed a null apparent activation energy, explaining the temperature insensitivity of the final acetylated silybin B (1b) concentration. Furthermore, the decrease in steady-state concentrations of the acetylated products with increasing volumetric flow rates indicated that the reaction was occurring in a kinetic regime. Interestingly, a maximum starting Sil concentration was identified, above which there was no favorable impact on conversion. Highlights: Silybin B was more selectively acetylated compared to silybin A. Reaction rate was insensitive to temperature due to exothermic adsorption. Kinetics and adsorption parameters were obtained by non-linear regression analysis. Good prediction achieved with axial dispersion model and Eley-Rideal mechanism. Flow chemistry boosts silibinin enzymatic resolution over traditional methods. [ABSTRACT FROM AUTHOR]

Objective: This study aimed to identify and characterize a novel endo-β-glucanase, IDSGLUC9-4, from the rumen metatranscriptome of Hu sheep. Methods: A novel endo-β-glucanase, IDSGLUC9-4, was heterologously expressed in Escherichia coli and biochemically characterized. The optimal temperature and pH of recombinant IDSGLUC9-4 were determined. Subsequently, substrate specificity of the enzyme was assessed using mixed-linked glucans including barley β-glucan and Icelandic moss lichenan. Thin-layer chromatography (TLC), high-performance liquid chromatography (HPLC), matrix assisted laser desorption ionization time of flight mass spectrometry analyses were conducted to determine the products released from polysaccharides and cello-oligosaccharides substrates. Results: The recombinant IDSGLUC9-4 exhibited temperature and pH optima of 40°C and pH 6.0, respectively. It exclusively hydrolyzed mixed-linked glucans, with significant activity observed for barley β-glucan (109.59±3.61 μmol/mg min) and Icelandic moss lichenan (35.35±1.55 μmol/mg min). TLC and HPLC analyses revealed that IDSGLUC9-4 primarily released cellobiose, cellotriose, and cellotetraose from polysaccharide substrates. Furthermore, after 48 h of reaction, IDSGLUC9-4 removed most of the glucose, indicating transglycosylation activity alongside its endo-glucanase activity. Conclusion: The recombinant IDSGLUC9-4 was a relatively acid-resistant, mesophilic endo-glucanase (EC 3.2.1.4) that hydrolyzed glucan-like substrates, generating predominantly G3 and G4 oligosaccharides, and which appeared to have glycosylation activity. These findings provided insights into the substrate specificity and product profiles of rumen-derived GH9 glucanases and contributed to the expanding knowledge of cellulolytic enzymes and novel herbivore rumen enzymes in general. [ABSTRACT FROM AUTHOR]

• Investigating Bipolaris maydis interaction with maize genotypes revealed varying levels of resistance and susceptibility. • Scanning electron microscopy showed stomatal pattern variations, correlating with mycelium invasion and symptom severity. • ABA quantification during infection showed lower ABA levels in resistant varieties, linked to a balanced defense response. • Resistant variety S-2022-11356 showed multiple mechanisms: physical barriers, reduced mycelium, unique stomata, and lower ABA levels. • Findings are significant for breeding programs and managing foliar diseases, emphasizing strategies for enhanced maize resistance. Bipolaris maydis is a prominent pathogen causing maydis leaf blight disease (MLB) in warm, humid regions worldwide. Structural components of plants, particularly stomata, play a crucial role in defending against pathogen invasion. In this study, we conducted a comprehensive investigation of stomatal interactions at the histopathological and molecular levels in various cultivated maize genotypes from Punjab state of India. Bipolaris maydis was isolated, purified, and inoculated onto six maize genotypes. Leaf samples were collected 48 h post-inoculation, representing the disease phase. Stomatal aperture bioassays and scanning electron microscopy (SEM) were performed on infected and non-infected samples. SEM analysis revealed distinct morphological variations, including stomatal aperture patterns and MLB pathogen invasion routes through stomata. Stomatal diameter varied among genotypes, and mycelium presence on the leaf surface was observed, with varying degrees of invasion through stomata. Genotypes exhibiting greater field symptom visibility displayed higher mycelium abundance and invasion. Additionally, high-performance liquid chromatography (HPLC) was employed to quantify abscisic acid (ABA) content in maize leaves during the Bipolaris maydis -maize interaction. This analysis aimed to elucidate the relationship between ABA and biotic stress, shedding light on its role in defense responses against the pathogen. Overall, our study enhances the understanding of stomatal interactions, surface morphology, and ABA dynamics in maize- Bipolaris maydis interactions. These findings have implications for breeding programs seeking to develop resistant maize varieties and contribute to the overall management of MLB disease. These findings provide valuable insights for future breeding programs targeting resistance against maize pathogens. [ABSTRACT FROM AUTHOR]

The present study evaluated modified solvent evaporation-assisted methanolic Mentha extracts for their antifungal efficacy against Phytophthora infestans. Mentha extracts showed significantly (p < 0.05) higher total tannin content (2193.5 ± 7.5 mg) in the root extract of Mentha citrate , followed by total flavonoid content (1777± 8 mg) in the leaf extract of Mentha piperta and total phenolic content (1710±4 mg) in the leaf extract of Mentha piperta. A significant amount of variability was found for bioactive compounds in Mentha varieties by using qualitative descriptors. Statistically, Mentha extracts and artificial antioxidants showed a significant (p < 0.05) difference in terms of percentage inhibition during DPPH, nitric acid scavenging, reducing power, phosphomolybdenum, chelating power, and hydroxyl radical scavenging assays, from which it was observed that the leaves, stem, and root of wild Mentha showed better antioxidant values. During the antifungal assay, the leaf extract of wild Mentha showed a significantly (p < 0.05) higher inhibition percentage, i.e., 33.2%, followed by the leaf extract of Mentha piperita , i.e., 31.9%. In contrast, the minimum percentage was found in Mentha arvensis (Kosi). Mentha varieties and ascorbic acid are also effective against P. infestans. The HPLC chromatogram of wild Mentha revealed a significantly (p < 0.05) higher eriocitrin level in the leaves, i.e., 7.92 mg, as compared to the stem i.e., 7.63 mg. This study identified Mentha as an alternative treatment against P. infestans as compared to traditional chemical pesticides and also reduced the impact of chemical pesticides on the environment. [Display omitted] • Eight Mentha varieties, i.e., Mentha arvensis (Unti), Mentha arvensis (Kranti), Mentha arvensis (Kosi), Mentha citrata (Kiran), Mentha piperita (Kukurel), Mentha spicata (Supriya), Mentha spicata L. Var. Viridis (MSS-5), and Wild Mentha were subjected to in vitro antifungal activity against P. infestans. • Phytochemical tests were performed for qualitative and quantitative analysis. • The inhibitory of 2,2-Diphenyl-1-picrylhydrazyl (DPPH), nitric oxide scavenging, reducing power, phosphomolybdenum assay, chelating power and hydroxyl radical scavenging assays were investigated, indicating antioxidant properties. • The extracts showed good antifungal activity against P. infestans, while leaf extract of wild Mentha gave the maximum inhibition percentage, i.e., 33.2 %. • High performance liquid chromatography (HPLC) revealed the presence of eriocitrin in the leaves and stem of wild Mentha. [ABSTRACT FROM AUTHOR]

• Lemon balm postdistillation waste extracts are abundant source of rosmarinic acid. • Antioxidant, antibacterial and anticholinesterase effects are pronounced. • Deodorized lemon balm leaves extracts possess the hepatoprotective effect. • Herbal-drug interaction with midazolam was recorded in rotarod performace test. • Lemon balm leaves extract reduce the levels of anxiety in experimental animals. Melissa officinalis L., Lamiaceae (lemon balm) leaves, essential oil and extracts have a long tradition of use. This aromatic plant is cultivated worldwide and there is a growing demand for its mass production. The aim of this study was to chemically characterize lemon balm postdistillation waste such are deodorized leaves, decoction remaining after the hydrodistillation of essential oil and stems and to determine whether waste extracts possess pharmacological activities comparable to standard lemon balm extract. The potential usage of postdistillation waste would be important for both ecological and economic reasons. Prepared waste extracts were chemically characterized regarding total phenolics and flavonoids and using high performance liquid chromatography for quantification of specific phenolic compounds. Antioxidant effect was examined ex vivo on liver homogenate of experimental animals. Pharmacodynamic studies included rotarod performance, tail suspension, elevated plus maze and novel object recognition tests and potential interactions between examined lemon balm extracts and midazolam, fluoxetine and diazepam. Rosmarinic acid was determined as a dominant compound in all investigated extracts ranging from 15.82 to 42.98 mg/g of dried extracts. Ex vivo , hepatoprotective effect of deodorized leaves extract was confirmed. Examined lemon balm extracts influenced the metabolism of midazolam without interacting with fluoxetine or diazepam, nor expressing the antidepressant effect or influencing the memory of treated animals. However, anxiolytic effect of lemon balm extracts was recorded. Postdistillation waste of lemon balm could be used as a potential source for pharmaceutical industry for the isolation of pharmacologically active compounds and production of herbal medicinal products. [ABSTRACT FROM AUTHOR]

A fullerene mixture was enriched with endohedral metallofullerenes (EMF) using Lewis acid (TiCl4), which took 22 min, whereas the standard method requires about 8 h. An algorithm for assessing small-area chromatographic peaks has been proposed, which has improved the accuracy of determination. For example, the area of the C84 peak was 4.24% using the developed program, while the use of chromatograph software estimated the area of this peak to be 1.78%. [ABSTRACT FROM AUTHOR]

Summary: Rosemary extract (RE) is a natural antioxidant, which has been widely used for preservation of oils. The main lipophilic components of RE are carnosic acid (CA) and carnosol (CN). However, the reports on the method for determining CA and CN in vegetable oils are really rare. Herein, a highly efficient method for quantitative analysis of CA and CN in vegetable oils was developed. The vegetable oil samples were dissolved in n‐hexane saturated using acetonitrile and extracted with acetonitrile saturated using n‐hexane, followed by HPLC analysis using UV detector. Qualitative and quantitative determinations were performed by external standard method. Under the optimised conditions, limit of detection (LOD) and limit of quantitation (LOQ) of CA were 0.11 μg mL−1 and 0.55 μg mL−1, respectively; LOD and LOQ of CN were 0.05 μg mL−1 and 0.20 μg mL−1, respectively. When the method was applied to determine CA and CN in vegetable oils spiked with standards, good recoveries (83.98% ~ 102.80% for CA and 98.29% ~ 114.74% for CN) and RSDs (0.61% ~ 7.36% for CA and 0.40% ~ 2.88% for CN, n = 2) were achieved. Accordingly, this work would efficiently identify and monitor lipophilic RE in vegetable oils, as this advanced method showed sensitive, quantitative, and reliable results suited for vegetable oils. [ABSTRACT FROM AUTHOR]

To construct a novel nano-carrier with dual ligands to achieve superior anti-tumour efficacy and lower toxic side effects. Liposomes were prepared by thin film hydration method. Ultraviolet, high performance liquid chromatography, nano-size analyser, ultrafiltration centrifugation, dialysis, transmission electron microscope, flow cytometry, Cell Counting Kit-8, confocal laser scanning microscopy, transwell, and tumorsphere assay were used to study the characterisations, cytotoxicity, and in vitro targeting of dg-Bcan targeting peptide (BTP-7)/pHA-temozolomide (TMZ)/tetra(4-carboxyphenyl)porphyrin (TCPP)-Lip. BTP-7/pHA-TMZ/TCPP-Lip was a spheroid with a mean diameters of 143 ± 3.214 nm, a polydispersity index of 0.203 ± 0.025 and a surface charge of −22.8 ± 0.425 mV. The drug loadings (TMZ and TCPP) are 7.40 ± 0.23% and 2.05 ± 0.03% (mg/mg); and the encapsulation efficiencies are 81.43 ± 0.51% and 84.28 ± 1.64% (mg/mg). The results showed that BTP-7/pHA-TMZ/TCPP-Lip presented enhanced targeting and cytotoxicity. BTP-7/pHA-TMZ/TCPP-Lip can specifically target the tumour cells to achieve efficient drug delivery, and improve the anti-tumour efficacy and reduces the systemic toxicity. [ABSTRACT FROM AUTHOR]

This study presents the results of aflatoxin contamination of maize and groundnuts in major markets in Accra and assesses the population's exposure to aflatoxins. Raw maize and groundnuts from 6 major markets in Accra were sampled and analysed for their aflatoxin content. A total of 92 samples comprising 48 maize and 44 groundnuts were analysed using high-performance liquid chromatography, after extraction with methanol/water and cleanup on an immunoaffinity column. Total aflatoxins were quantified in 98% of the maize samples and 70% of the groundnut samples, with concentrations ranging from 0.60 to 1065 µg/kg and 0.20 to 627 µg/kg, respectively. Exposure assessment showed an estimated daily intake of 0.436 μg/kg bw/day and 0.0632 μg/kg bw/day for maize and groundnut consumption, respectively, suggesting significant health risks for consumers. The high prevalence and concentrations of aflatoxins call for an urgent need for measures to control exposure of the Ghanaian population. [ABSTRACT FROM AUTHOR]

The applicability of two layered double hydroxide adsorbents, that is, Zn/Al LDH and the reduced graphene oxide-modified Zn/Al-rGO LDH for the solid phase extraction-preconcentration of naproxen followed by HPLC determination is evaluated and compared. The adsorbents are characterized by using XRD, FT-IR, FE-SEM, BET, and TEM techniques. The optimization of parameters affecting the extraction procedure included pH and sample solution volume, amount of the adsorbents, adsorbent/sample solution contact time, type, concentration, and volume of the desorption solution, and the time required for desorption process was performed by using univariate method. It is assumed that the uptake of anionic form of naproxen is taken place via the ion exchange mechanism with interlayer carbonate anions of the studied LDHs. The applicability of the adsorbents is evaluated by the determination of naproxen in human urine, hospital, and pharmaceutical wastewater samples. The obtained linear ranges by employing the unmodified and modified LDHs for the determination of naproxen in pharmaceutical wastewater were found to be 10–530 µg L−1 (R2 = 0.9999) and 5–630 µg L−1 (R2 = 0.9999), respectively. The limits of detection and enrichment factor were appraised as 5.1 µg L−1 and 42 by employing Zn/Al LDH, and 3.1 µg L−1 and 54.5 by using Zn/Al-rGO LDH. Both investigated LDHs are able to be used in solid phase extraction-preconcentration of naproxen in real samples. However, the evaluated figures of merit reveal that the modified Zn/Al-rGO LDH is more efficient adsorbent than the unmodified Zn/Al LDH for the extraction of naproxen. [ABSTRACT FROM AUTHOR]

Capparis masaikai Lévl is a Chinese native plant that ripe seeds are often used as a traditional Chinese medicine for their heat antidotes properties. The locals like to chew the seeds for their distinctive flavor "sweet water taste". In this study, enzymatic hydrolysis, gel filtration chromatography, and reversed-phase high-performance liquid chromatography were used to extract, isolate and purify flavor peptides from the seed kernels of Capparis masaikai Lévl. Nano-LC−MS/MS was used to identify 219 peptides in total. Five new bitter peptides (HIGP, FHP, CFR, LYR and SFR) were screened by molecular docking. The results of molecular docking indicated that hydrogen bonds and hydrophobic bonds played essential roles in the binding of the five bitter peptides to T1R2-T1R3, T2R1 and T2R34. Phe75 and Glu74 on T2R1 and Arg373 on T1R2-T1R3 might be the critical amino acids in the binding site. The taste properties of the synthesized peptides were confirmed by sensory evaluation, and it was found that five peptides exhibited a specific sweetness inhibition. Not only do these results shed light on the interaction between flavor peptides and taste receptors, but they also help explain the "sweet water taste" of the seed kernels of Capparis masaikai Lévl. The results of this study help to explore the potential of flavor peptides in an enzymatic hydrolysate of Capparis masaikai Lévl seed kernels and broaden the diversity of flavor sources for the "sweet water taste". [ABSTRACT FROM AUTHOR]

Capsanthin is a natural red–orange pigment present in red paprika and has been proven to have various health benefits. The rising consumption of chili peppers and the global demand of natural color promote the need for capsanthin quantification analysis. In the present study, a high-performance liquid chromatography method was developed for the analysis of capsanthin in chili peppers and their products. The chromatographic and extraction parameters were optimized. The concentration of capsanthin ranged from 0.5 to 200 mg/L which showed good linearity (R2 > 0.99). The LOD and LOQ of samples ranged from 0.014 to 0.092 mg/kg and 0.049–0.12 mg/kg, respectively. The recovery experiment (recovery rate 84.79–103.55%, RSD 1.64–9.27%) and interlaboratory test (the RSD of repeatability and reproducibility was in the range of 3.11–4.06% and 4.66–5.52%, respectively) demonstrated good accuracy, precision, repeatability, and reproducibility of the proposed method. The results indicate that the developed method will be a valuable tool for routine analysis of capsanthin in chili peppers and their products. [ABSTRACT FROM AUTHOR]

This study was intended to determine the melissopalynological characteristics, LAB color, browning index, total phenolic content, antioxidant activity, phenolic profile, and their correlations within Iranian honeys. Ten honey samples were collected from beekeepers in various floristic regions of Iran, along with two commercial multi-floral samples. To determine the antioxidant activity, three methods of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging, β-carotene bleaching, and Ferric reducing/antioxidant power (FRAP) were used. Phenolic compounds were analyzed by high-performance liquid chromatography with diode-array detection (HPLC–DAD). Pollen analysis revealed that bees primarily fed on the Fabaceae and Asteraceae families in the Iranian flora. The local samples were taxonomically categorized as multi-floral honey. Besides, the commercial samples demonstrated the lowest levels of total phenolics and relatively poor antioxidant activity across all three methods. Syringic acid and luteolin were the predominant phenolic compounds in all samples. A strong correlation (p < 0.01) was found between color, melanoidin content and antioxidant activity, while no significant correlation existed between phenolic content and antioxidant activity. Overall, the results confirmed that examined multi-floral honeys exhibited inferior antioxidant activity compared to studies conducted in other regions worldwide, possibly due to sugar-fed bees, insufficient levels of potent phenolic constituents, and post-harvest thermal treatments. [ABSTRACT FROM AUTHOR]

This study utilizes a novel green chemistry method to synthesize aryl-substituted dihydropyrimidone derivatives (P1-P7), with structural information determined through various analytical techniques, including IR, 1H-NMR, HPLC, GCMS, and CHNS elemental analysis. The photophysical properties of the synthesized molecules were assessed using the DFT-B3LYP-6-31G(d) basis set within the Gaussian-09w software. The molecule P1 shows the highest bandgap of 4.497eV. The GCRD parameters reveal the high electrophilic behavior of P4 and P5. The general findings derived from the GCRD parameter indicate that the synthesized molecules exhibit a pronounced reactivity. Furthermore, the synthesized molecules were evaluated for antibacterial and antifungal activities, demonstrating that P4 and P5 exhibit heightened reactivity against S. typhi, E. coli, A. niger, and C. albicans. [ABSTRACT FROM AUTHOR]

Objective Conventional imaging of cancer with modalities such as computed tomography or magnetic resonance imaging provides little information about the underlying biology of the cancer and consequently little guidance for systemic treatment choices. Accurate identification of aggressive cancers or those that are likely to respond to specific treatment regimens would allow more precisely tailored treatments to be used. The expression of the estrogen receptor α subunit is associated with a more aggressive phenotype, with a greater propensity to metastasize. We aimed to characterize the binding properties of an 18 F-estradiol positron emission tomography (PET) tracer in its ability to bind to the α and β forms of estrogen receptors in vitro and confirmed its binding to estrogen receptor α in vivo. Methods The 18 F-estradiol PET tracer was synthesized and its quality confirmed by high-performance liquid chromatography. Binding of the tracer was assessed in vitro by saturation and competitive binding studies to HEK293T cells transfected with estrogen receptor α (ESR1) and/or estrogen receptor β (ESR2). Binding of the tracer to estrogen receptor α in vivo was assessed by imaging of uptake of the tracer into MCF7 xenografts in BALB/c nu/nu mice. Results The 18 F-estradiol PET tracer bound with high affinity (94 nM) to estrogen receptor α, with negligible binding to estrogen receptor β. Uptake of the tracer was observed in MCF7 xenografts, which almost exclusively express estrogen receptor α. Conclusion 18 F-estradiol PET tracer binds in vitro with high specificity to the estrogen receptor α isoform, with minimal binding to estrogen receptor β. This may help distinguish human cancers with biological dependence on estrogen receptor subtypes. [ABSTRACT FROM AUTHOR]

The increasing use of UV filters, such as benzophenone-3 (BP-3) and titanium dioxide nanoparticles (TiO2 NPs), has raised concerns regarding their ecotoxicological effects on the aquatic environment. The aim of the present study was to examine the embryo-larval toxicity attributed to BP-3 or TiO2 NPs, either alone or in a mixture, utilizing zebrafish (Danio rerio) as a model after exposure to environmentally relevant concentrations of these compounds. Zebrafish embryos were exposed to BP-3 (10, 100, or 1000 ng/L) or TiO2 NPs (1000 ng/L) alone or in a mixture (BP-3 10, 100, or 1000 ng/L plus 1000 ng/L of TiO2 NPs) under static conditions for 144 hr. After exposure, BP-3 levels were determined by high-performance liquid chromatography (HPLC). BP-3 levels increased in the presence of TiO2 NPs, indicating that the BP-3 degradation decreased in the presence of the NPs. In addition, in the presence of zebrafish, BP-3 levels in water decreased, indicating that zebrafish embryos and larvae might absorb BP-3. Data demonstrated that, in general, environmentally relevant concentrations of BP-3 and TiO2 NPs, either alone or in a mixture, did not significantly induce changes in heart and spontaneous contractions frequencies, levels of reactive oxygen species (ROS), morphological and morphometric parameters as well as mortality rates during 144 hr exposure. However, the groups exposed to TiO2 NPs alone and in a mixture with BP-3 at 10 ng/L exhibited an earlier significant hatching rate than the controls. Altogether, the data indicates that a potential ecotoxicological impact on the aquatic environment exists. [ABSTRACT FROM AUTHOR]

Background: The pancreas contains Vitamin D (Vit.-D) and an enzyme that regulates insulin levels. Vitamin D deficiency is associated with several severe health conditions, such as cardiovascular disease, diabetes, various cancers, and multiple sclerosis (MS). Therefore, the objective of the current study is to investigate the correlation between Vitamin D levels and glycosylated hemoglobin (HbA1c) in both patients and controls. Materials and Methods: The study enrolled 163 T2DM (Group I) and 174 healthy (Group II) subjects to estimate the level of Vit.-D and HbA1c in the blood serum of all subjects, using radioimmunoassay and high-performance liquid chromatography, respectively. Results: The results revealed that Group I had a lower level of Vit.-D (17.82 ± 2.23 ng/mL) than Group II. Similarly, they have high HbA1c levels, showing significant (P < 0.001; Student's t -test). Further, in Group I, Vit.-D levels were negatively correlated with HbA1c levels (P < 0.001; r2 = 0.07, linear regression). Group I and II combined analysis revealed an inverse relationship between Vit.-D levels and HbA1c (P < 0.001; r2 = 0.021). Conclusion: The study concluded a negative correlation between Vit.-D levels and HbA1c levels in T2DM. However, Vit.-D therapy can recover this correlation, which helps control glycemic levels. [ABSTRACT FROM AUTHOR]

A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. Chromatographic separation was achieved with C18 (5 µm × 4.6 mm × 150 mm) column, at 30 °C with isocratic elution, mobile phase composed of solution A (acetonitrile), and solution B (0.5% formic acid) (65:35 v/v) at flow rate 1.2 mL min−1. The linearity range is 10–150 ng mL−1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. The retention time is 8.20 ± 0.02 min. LOD is found to be 3.3 ng mL−1 for drug. The method was applied to the analysis of SLP in human plasma with good recovery as 97.83%. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a prototype pharmacokinetic study by administration of 800 μg SLP to a healthy volunteer and parameters like AUC0–24, AUC0–∞, Cmax, tmax, and t1/2 were assessed. [ABSTRACT FROM AUTHOR]

A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank. [ABSTRACT FROM AUTHOR]

Pinus merkusii Jungh & De Vries. has become increasingly gathered more attention from researchers because the plant has a range of folk medicinal uses. Heartwood plant is the major source of dehydroabietic acid (DHAA) and abietic acid (AA), which possesses several medicinal properties, such as antiviral, antimicrobial, antiobesity and anti-inflammatory. The research proposed herein a low-cost, fast, specific, uncomplicated, sensitive, precise reverse-phase high-performance liquid chromatography (RP-HPLC). This method was conducted and validated for evaluating an amount of DHAA and AA in ethanol extract and oral spray containing P. merkusii heartwood extract. Additionally, stability and antimicrobial activities against clinically isolated Streptococcus mutans of the oral spray were determined. The separation was achieved on Pursuit 200Å PFP column, 150 × 4.6 mm, particles of 3 µm with a flow rate of 1.0 mL min−1. Methanol and water (70:30 v/v) were used as eluent with an isocratic mode and sample analysis volume was set at 10 µL, at a detection wavelength of 210 and 245 nm. The developed HPLC method for analysis of DHAA and AA showed good linearity with correlation coefficients equal to 1. Moreover, other validation parameters, comprised of accuracy, precision, specificity and detection and quantitation limits of this method displayed excellent reliability, validity and sensitivity. This method could be an interesting alternative for quantitative measurement of P. merkusii heartwood extract, oral spray formulation and other P. merkusii heartwood extract preparations. The result from antibacterial tests suggested that the oral spray containing P. merkusii heartwood extract is able to inhibit the oral pathogens causing dental caries. The oral spray decreased S. mutans population size by about 0.5–2 Log CFU mL−1 at 1–4 h and complete elimination of all bacteria strains within 24 h. This study provides validity for using P. merkusii heartwood extract as an alternative for preventing and treating oral infectious diseases. [ABSTRACT FROM AUTHOR]

The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R 2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument. [ABSTRACT FROM AUTHOR]

Purpose: To protect and improve the soil environment of the Songnen Plain, detailed identification of organic pollutant contamination features in the soil and the degree of contamination is required. The primary goals of this research are to measure the levels of organic pollutants detected in the soil of the Songnen Plain, to correlate the levels of organic pollutants with different land use practices, and to assess the environmental quality of the soil using various pollution indicators. Material and methods: Contaminated soil was collected at three types of areas: residential (n = 26), agricultural (n = 22), and industrial (n = 12) in the Songnen Plain of Jilin Province, at 0–20 cm and 20–40 cm depths. The concentrations of dichlorodiphenyltrichloroethane, benzene hexachloride, toluene, ethylbenzene, xylene, benzo (a) pyrene (BaP), trichloromethane, tetrachloromethane, hexachlorobenzene, and atrazine in the soil samples were determined using gas chromatography (GC), gas chromatograph-mass spectrometer-mass spectrometer (GC-MS-MS), and high-performance liquid chromatography (HPLC). Results and discussion: Soil BaP had the highest concentration with a mean value of 20.59 ng/kg, followed by atrazine, hexachlorobenzene, benzene hexachloride, dichlorodiphenyltrichloroethane (DDT), trichloromethane, toluene, ethylbenzene, xylene, and tetrachloromethane with mean concentrations of 0.46, 0.44, 0.34, 0.28, 0.21, 0.14, 0.06, 0.03, and 0.02 ng/kg, respectively. Soil organic pollutants at all sampling sites did not exceed the secondary environmental quality standard values. The most serious soil contamination was found in landfill sites, followed by urban areas, industrial areas and farmland areas. Conclusions: Soil contamination is more severe in locations where human activity is more prevalent. The subsoil can better reflect the characteristics of soil pollution in the area compared to the upper layer of soil. Although contamination is low in the research region, the presence of these pollutants must be taken seriously in order to maintain the quality and safety of agricultural products and human health. [ABSTRACT FROM AUTHOR]

Copyright of Chinese Journal of Inorganic Analytical Chemistry / Zhongguo Wuji Fenxi Huaxue is the property of Beijing Research Institute of Mining & Metallurgy Technology Group and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

This study aimed to elucidate the potential of Pseudomonas species to degrade furfuryl alcohol (FA), a widely used furanic compound. FA-based resins and biopolymers have applications in various sectors, leading to the gradual discharge of FA into the environment through industrial wastewater. The objective was to find an eco-friendly solution for removing FA residues from industrial effluents, thereby eliminating the hazardous effects of FA. Pseudomonas species have emerged as potential bacterial genera for biodegradation of aromatic compounds; therefore, this study examined the effectiveness of Pseudomonas putida MTCC 1194 and Pseudomonas aeruginosa MTCC 1034 for FA degradation. Significant shifts in the fingerprint regions were observed using Fourier-transform infrared (FTIR) spectroscopy, providing evidence of successful FA degradation. A more than 50% reduction in FA content was observed by both strains, even at high concentrations (500 mgl− 1), as determined by spectrophotometric and high-performance liquid chromatography (HPLC) analysis. Liquid chromatography-mass spectrometry (LC-MS) identified the metabolite as 2-furoic acid (113 m/z). Both bacterial cultures followed substrate inhibition kinetics, and the specific growth rate best fit the Aiba and Haldane models for P. putida and the Haldane and Edwards models for P. aeruginosa. Furthermore, immobilized bacterial cells maintained approximately 50% FA degradation (300 mgl− 1) over five degradation cycles, highlighting their stability and reusability. The phytotoxicity bioassay demonstrated the non-hazardous nature of the metabolites formed after FA biodegradation. These findings underscore the potential of these strains for effective FA bioremediation, paving the way for their use in industrial effluent treatment. [ABSTRACT FROM AUTHOR]

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Polyaromatic Hydrocarbons (PAHs) in the environment have been linked to severe health effects. This study aims to assess the atmospheric pollutant and analyze the variation in PAHs, focussed on benzo[a]pyrene [B(a)P]. Among all PAHs, B(a)P is regarded as a marker for human carcinogenicity. This study reflects the B(a)P concentration and its correlation with the particulate matter (PM10 and PM2.5) in rural, peri-urban, and urban areas of Panvel Municipal Corporation, Maharashtra, India. Samples were collected during the pre & post-monsoon season for two consecutive years (Yr. 2020 and Yr. 2021). B(a)P level was determined using high-performance liquid chromatography coupled with a diode array detector. It was observed that PM2.5 and PM10 show a strong positive correlation (r=0.8-0.9) with B(a)P. It is observed that B(a)P concentrations were high in pre-monsoon w.r.t. post-monsoon, and this concentration increased spatially as we moved from rural to urban areas. Pre-monsoon B(a)P concentration varies somewhat by 5% between rural to urban areas as compared to post-monsoon. High levels of vehicular emissions and industry were associated with the distribution of B(a)P in urban areas, whereas a combination of local emissions and metropolitan area diffusion was responsible for the presence of B(a)P in peri-urban and rural areas. Also, this study captures the variation of B(a)P levels during the period of COVID-19. In future studies, Artificial Intelligence (AI) can augment the determination of PAHs in soil by improving the accuracy and speed of analysis using predictive modeling based on different input parameters to determine outliers in soil PAH data, building sensor networks for real-time monitoring of PAH levels, leverage robotics for automated sample preparations, and rapid testing of samples to identify hotspots. [ABSTRACT FROM AUTHOR]

Nineteen cannabinoids, including Δ9-THC (tetrahydrocannabinol) and CBD (cannabidiol), were quantified in 22 CBD oils, 2 CBG (cannabigerol) oils, and 2 CBN (cannabinol) oils, marketed as food supplements, aroma oils, or cosmetic preparations. Analyses were conducted using high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The declared concentrations of CBD (or CBG, CBN) in the oils ranged from 2.5 to 20%. Actual concentrations compared to declared concentrations ranged from 81 to 226%. CBD concentrations of up to 9 mg per drop were found. Δ9-THC was detected in 20 of 26 samples, with concentrations ranging from 5 to 1576 mg/kg (mean = 536 mg/kg). Considering the highest daily intake suggested by one manufacturer (20 drops) and a body weight of 70 kg, the measured Δ9-THC concentration in 50% (n = 13) of the products would exceed the acute reference dose (ARfD) of 1 µg/kg body weight (bw) derived for Δ9-THC by the European Food Safety Authority (EFSA). For 7 samples, only 2 drops of oil would be sufficient to exceed the ARfD of Δ9-THC. [ABSTRACT FROM AUTHOR]

This article discusses a study on the effects of metabolic and bariatric surgery (MBS) on neonatal birth weight in women with polycystic ovary syndrome (PCOS) and high body mass index (BMI). The study found that the length of pregnancy was the only factor associated with newborn weight, regardless of PCOS status. Factors such as weight gain during pregnancy and nutritional variables did not have a significant effect on newborn weight. The study suggests that MBS may be an effective treatment for women with PCOS and high BMI seeking fertility. [Extracted from the article]

Prepregs are highly dependent on the resin, its chemical composition, and physical properties. Resin is the perishable part of prepreg materials and usually requires controlled storage, otherwise, its processability and properties may be affected. Oven curing prepregs are recognized to have longer life out of the freezer than those designed to cure in autoclave, and one of them, prepreg 2511, is the focus of this research. Prepreg 2511 has a formal out-time limit of 28 days at clean room environment (23°C/50% relative humidity), and 24 months shelf life, when frozen at −18°C, while common prepreg designed to be cured in autoclave, usually have 15 days of out-time and 12 months of shelf-life. It is known that the real shelf life and out time of epoxy-based materials tends to be longer than suppliers' recommendation. Aiming to assess 2511 performance after those 28 days of exposure to clean room ambient, during and after 24 months in freezer; the material was exposed to this environmental condition for more than 28 days and tested periodically using different methods, including, Differential Scanning Calorimeter, High-Performance Liquid Chromatography tack, among others. In resume, the goal of this research was to identify 2511 longest out life without losing its properties and which of the tests used during these experiments would be more sensitive to capture its aging. [ABSTRACT FROM AUTHOR]

Rationale: Cloxacillin and flucloxacillin are prone to degradation and polymerization in humid and hot environments, and their polymers have long been recognized to trigger allergic manifestations. A series of the degradation and polymerized impurities in cloxacillin and flucloxacillin were separated and characterized to ensure safe use of these drugs by the public. Methods: By studying the chromatographic behavior of the degradation impurities and polymerized impurities in reversed‐phase high‐performance liquid chromatography (RP‐HPLC) gradient elution, the impurities in cloxacillin and flucloxacillin were effectively separated and eluted. RP‐HPLC tandem ion trap/time‐of‐flight mass spectrometry (MS) was applied to characterize the structures of unknown impurities eluted from the RP‐HPLC methods for cloxacillin and flucloxacillin. The mechanisms of formation of the impurities in cloxacillin and flucloxacillin were also investigated. Results: The structures of 10 unknown impurities in cloxacillin and 8 unknown impurities in flucloxacillin were elucidated based on the high‐resolution MSn data at positive and negative modes, respectively. Six polymerized impurities were found and characterized, of which three were from the polymerization of cloxacillin and three were from the polymerization of flucloxacillin. Conclusions: The study on the impurity profiles of cloxacillin and flucloxacillin provided a scientific basis for improving their production processes and quality control. [ABSTRACT FROM AUTHOR]

BACKGROUND: Gluten composition is an important quality parameter of wheat flour. Reversed‐phase high‐performance liquid chromatography (RP‐HPLC) is a state‐of‐the‐art method for its analysis. As this is a very labour‐intensive and time‐consuming procedure, alternative faster methods are desirable. Enzyme‐linked immunosorbent assay (ELISA) is a high‐throughput method often used for the analysis of gluten traces in gluten‐free products. In this proof‐of‐principle study, we introduce an experimental triple ELISA for the relative quantitation of gliadins, high‐molecular‐weight glutenin subunits (HMW‐GS) and low‐molecular‐weight glutenin subunits (LMW‐GS) of one wheat flour extract. RESULTS: The results of 80 common wheat flour samples obtained from the triple ELISA and RP‐HPLC were correlated. The results for gliadins (r = 0.69) and HMW‐GS (r = 0.81) showed a medium and high correlation, respectively. Only a very weak correlation of ELISA and RP‐HPLC results was observed for LMW‐GS (r = 0.49). Results for glutenins (r = 0.69) and gluten (r = 0.72) had a medium correlation. The gliadin/glutenin ratio (r = 0.47) and LMW‐GS/HMW‐GS ratio (r = 0.40) showed a weak or no correlation. The gliadin, LMW‐GS and gluten contents were lower and the HMW‐GS content was higher in the ELISA measurement compared to RP‐HPLC. CONCLUSION: The quantitation of gliadins and HMW‐GS by the experimental triple ELISA showed comparable results to RP‐HPLC, whereas no strong correlation between the results from the two methods was found for LMW‐GS. Overall, the experimental triple ELISA is suitable for relative gluten quantitation, especially for the analysis of large sample sets. Further work will focus on improving the experimental procedure of the ELISA. © 2024 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. [ABSTRACT FROM AUTHOR]

AbstractIn this dual-center study, we assessed the BioHermes A1C EXP M13 system for point-of-care (POC) HbA1c testing against two NGSP-certified HPLC instruments, the Bio-Rad D100 and Tosoh G8. Analyzing 605 samples, we evaluated the A1C EXP's reproducibility, sensitivity, specificity and impact of anemia on HbA1c measurements. The device showed excellent reproducibility with CVs under 2.4% and high sensitivity and specificity for diabetes diagnosis—98.1% and 96.8% against D100, and 97.1% and 96.7% against G8. Passing-Bablok regression confirmed a close correlation between A1C EXP and the HPLC instruments, with equations y = 0.10625 + 0.9688x (D100) and y = 0.0000 + 0.1000x (G8), and Bland–Altman plots indicated mean relative differences of −1.4% (D100) and −0.4% (G8). However, in anemic samples, A1C EXP showed a negative bias compared to HPLC devices, suggesting that anemia may affect the accuracy of HbA1c results. The study indicates that A1C EXP is a reliable POC alternative to laboratory assays, albeit with considerations for anemic patients. [ABSTRACT FROM AUTHOR]