Liquid Extraction Research Articles

Revolutionizing Dye Removal: Unleashing the Power of Liquid–Liquid Extraction Batch Process

Revolutionizing Dye Removal: Unleashing the Power of Liquid–Liquid Extraction Batch Process

Phyto-Photodynamic Therapy of Prostate Cancer Cells Mediated by Yemenite 'Etrog' Leave Extracts.

Cancer therapy, from malignant tumor inhibition to cellular eradication treatment, remains a challenge, especially regarding reduced side effects and low energy consumption during treatment. Hence, phytochemicals as cytotoxic sensitizers or photosensitizers deserve special attention. The dark and photo-response of Yemenite 'Etrog' leaf extracts applied to prostate PC3 cancer cells is reported here. An XTT cell viability assay along with light microscope observations revealed pronounced cytotoxic activity of the extract for long exposure times of 72 h upon concentrations of 175 μg/mL and 87.5 μg/mL, while phototoxic effect was obtained even at low concentration of 10.93 μg/mL and a short introduction period of 1.5 h. For the longest time incubation of 72 h and for the highest extract concentration of 175 μg/mL, relative cell survival decreased by up to 60% (below the IC50). In combined phyto-photodynamic therapy, a reduction of 63% compared to unirradiated controls was obtained. The concentration of extract in cells versus the accumulation time was inversely related to fluorescence emission intensity readings. Extracellular ROS production was also shown. Based on an ATR-FTIR analysis of the powdered leaves and their liquid ethanolic extract, biochemical fingerprints of both polar and non-polar phyto-constituents were identified, thereby suggesting their implementation as phyto-medicine and phyto-photomedicine.

Allelopathic effect of the methanol extract of the weed species-red sorrel (Rumex acetosella L.) on the growth, phytohormone content and antioxidant activity of the cover crop - white clover (Trifolium repens L.)

Allelopathy is a biological process in which one organism releases biochemicals that affect the growth and development of other organisms. The current investigation sought to determine the allelopathic effect of Rumex acetosella on white clover (Trifolium repens) growth and development by using its shoot extract (lower IC50 value) as a foliar treatment. Here, different concentrations (25, 50, 100, and 200 g/L) of shoot extract from Rumex acetosella were used as treatments. With increasing concentrations of shoot extract, the plant growth parameters, chlorophyll and total protein content of Trifolium repens decreased. On the other hand, ROS, such as O2.− and H2O2, and antioxidant enzymes, including SOD, CAT, and POD, increased with increasing shoot extract concentration. A phytohormonal study indicated that increased treatment concentrations increased ABA and SA levels while JA levels were reduced. For the identification of allelochemicals, liquid‒liquid extraction, thin-layer chromatography, and open-column chromatography were conducted using R. acetosella shoot extracts, followed by a seed bioassay on the separated layer. A lower IC50 value was obtained through GC/MS analysis. gammaSitosterol was identified as the most abundant component. The shoot extract of Rumex acetosella has strong allelochemical properties that may significantly impede the growth and development of Trifolium repens. This approach could help to understand the competitive abilities of this weed species and in further research provide an alternate weed management strategy.

POF-based biosensors for cortisol detection in seawater as a tool for aquaculture systems

A surface plasmon resonance (SPR) phenomenon implemented via D-shaped polymer optical fiber (POF) is exploited to realize cortisol biosensors. In this work, two immonosensors are designed and developed for the qualitative as well as quantitative measurement of cortisol in artificial and real samples. The performances of the POF-based biosensors in cortisol recognition are achieved using different functionalization protocols to make the same antibody receptor layer over the SPR surface via cysteamine and lipoic acid, achieving a limit of detection (LOD) of 0.8 pg/mL and 0.2 pg/mL, respectively. More specifically, the use of cysteamine or lipoic acid changes the distance between the receptor layer and the SPR surface, improving the sensitivity at low concentrations of about one order of magnitude in the configuration based on lipoic acid. The LODs of both cortisol biosensors are achieved well competitively with other sensor systems but without the need for amplification or sample treatments. In order to obtain the selectivity tests, cholesterol and testosterone were used as interfering substances. Moreover, tests in simulated seawater were performed for the same cortisol concentration range achieved in buffer solution to assess the immunosensor response to the complex matrix. Finally, the developed cortisol biosensor was used in a real seawater sample to estimate the cortisol concentration value. The gold standard method has confirmed the estimated cortisol concentration value in real seawater samples. Liquid–liquid extraction was implemented to maximize the response of cortisol in liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) analysis.

Unique Selectivity Reversal in the Complexation of Uranium(VI) and Plutonium(IV) with Two Novel C-Pivoted Tripodal Amide Ligands: Extraction and Liquid Membrane Transport Studies

ABSTRACT Two new carbon pivoted tripodal amide-containing ligands with different spacers (L I : -CH2- spacer; L II : -CH2-CH2- spacer) have been investigated for the liquid–liquid extraction of tetravalent plutonium and hexavalent uranium from nitric acid feed solutions. The studies were carried out using the ligand solutions prepared in 95% n-dodecane + 5% isodecanol. Pu(IV) extraction was higher than that of U(VI) at 3 M HNO3 for ligand L I which was just the opposite for ligand L II . Increase of the nitric acid concentration resulted in increasing extraction of both metal ions. Isodecanol variation studies exhibited decrease in the extraction of Pu(IV) and U(VI) with increasing isodecanol content in the organic phase. Greater that 98% stripping of Pu(IV) and U(VI) was obtained from the complexes of L I and L II using 0.5 M HNO3 + 0.1 M HEDTA and 1 M Na2CO3, respectively. The slope analysis study suggested the formation of 1:2 (ML2) species with Pu(IV) as well as U(VI) with both ligands at 3 M HNO3. Temperature variation studies showed that the extraction of U(VI) and Pu(IV) with both ligands is exothermic in nature. Supported liquid membrane transport experiments using 0.11 M ligands (L I and L II ) in 95% n-dodecane + 5% isodecanol indicated poor transport (<10% after 2 h) of U(VI) and Pu(IV).

A facile method to fabricate sustainable bamboo ethanol lignin/carboxymethylcellulose films with efficient anti-ultraviolet and insulation properties

Given the environmental concerns related to the non-degradability of conventional petroleum-based polymer films, the synthesis of biodegradable films utilizing natural polymers derived from biomass has emerged as a promising alternative, garnering significant attention in recent research endeavors. This research introduced an environmentally friendly and efficient method, utilizing extract liquid from the green ethanol pulping process as the solvent to completely dissolve carboxymethylcellulose into the film-forming liquid, and employing the solution pouring technique to successfully fabricate bamboo ethanol lignin/carboxymethylcellulose films (LCF). The findings revealed that the lignin content significantly influenced the LCF, endowing them with tunable mechanical properties, effective UV-blocking, and thermal insulation capabilities. With a lignin addition of 3.75 %, LCF-3.75 exhibited enhanced mechanical properties, characterized by a tensile strength of 19.4 MPa, along with superior UV-blocking efficiency, blocking 100 % of UVB and 99.81 % of UVA rays. Furthermore, relative to LCF-0, LCF-3.75 had been shown to possess enhanced hydrophobicity and thermal stability, culminating in the development of the composite films that showcased exceptional thermal insulation properties and biodegradability. The films not only harbored extensive application prospects as an anti-ultraviolet and heat-insulating glass films but also represented a potential avenue for the efficient utilization of lignin, thereby contributing to sustainable development.

Chemical Compositions, Phytochemical Screenings and Antifungal Activities of Cashew Nut Shell Liquid Extracts on Phytopathogenic Fungi of Yam (Dioscorea rotundata)

This study was carried out to evaluate the antifungal activity of Cashew (Anacardium occidentale L.) nutshell liquid on fungal pathogens of dry rot diseases of yam (Dioscorea cayennensis subsp. rotundata). The Soxhlet extraction method was used and constituents were identified and quantified using Gas chromatography. Isolation and identification of fungi complexes associated with dry rot disease of yam were made using Potato dextrose agar (PDA) as a medium. The antifungal activity of CNSL was evaluated using the food poisoning technique on PDA at 25, 50, 75 and 100% concentrations of CNSL dissolved in dimethyl sulphoxide. Azulene (57.65%) was the major chemical component of CNSL with phenolic compounds; anacardol, cresols and anacardic acid, among other compounds. CNSL phytochemical screening showed the presence of flavonoids, alkaloids, saponins, tannins, phenols, terpenoids, volatile oil and steroids. Infected yam tubers were isolated, four fungal strains (Fusarium solani, Lasiodiplodia theobromae, Aspergillus fumigatus, and A. niger) were identified, and pathogenicity test confirmed the association of the fungi species with the dry rot disease of white yam. CNSL was active against the identified fungi and could potentially compete with conventional standard as a suitable fungicide against dry rot disease of white yam.

Upgrading/Deacidification of Bio-Oils by Liquid–Liquid Extraction Using Aqueous Methanol as a Solvent

Oxygenated compounds such as acids in bio-oils (BO) have been related to the corrosion of metals and their storage instability when applied as fuels. Therefore, upgrading BO by removing acids (deacidification) can be a valuable technique to reduce corrosivity using specific separation processes. Therefore, the objective of this paper was to evaluate the effect of the water content in the solvent (aqueous methanol), the carboxylic acid content in the BO and extraction temperature on the deacidification process by liquid–liquid extraction (LLE), as well as the effect of the same parameters on the quality of the deacidified BO through physical–chemical and GC-MS analyses. The results show that an increase in the water content (5 to 25%) in the solvent and an increase in the carboxylic acids content (24.38 to 51.56 mg KOH/g) in the BO reduce the solvent’s capacity to extract carboxylic acids while increasing the temperature (25 to 35 °C) of the deacidification process promoted an increase in its capacity to remove them. Consequently, the highest deacidification efficiency (72.65%) is achieved with 5% water in methanol at 25 °C for BO1 (TAN = 24.38 mg KOH/g). Therefore, the deacidification process through LLE using aqueous methanol contributed significantly to BO upgrading.

Phytochemical determination and mechanistic investigation of Polygala tenuifolia root (Yuanzhi) extract for bronchitis: UPLC-MS/MS analysis, network pharmacology and in vitro/in vivo evaluation

Ethnopharmacological relevanceBronchitis is a respiratory disease characterized by a productive cough. Polygala tenuifolia Willd., commonly known as Yuan zhi, is a traditional Chinese herbal medicine used for relieving cough and removing phlegm. Despite its historical use, studies are lacking on the effectiveness of P. tenuifolia in treating bronchitis. Furthermore, the molecular mechanisms underlying the action of its bioactive compounds remain unknown. Aim of the studyThis study aims to identify the main bioactive compounds responsible for the effects of P. tenuifolia liquid extract (PLE) in treating bronchitis and to elucidate the associated molecular mechanisms. Materials and methodsThe main chemical compounds in PLE were identified and determined using ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The antitussive, expectorant and anti-inflammatory activities of PLE were evaluated in an ammonia-induced mouse cough model, a tracheal phenol red excretion mouse model, and a xylene-induced ear swelling mouse model, respectively. A network pharmacology analysis was conducted to investigate the associated gene targets, gene ontology, and KEGG pathways related to the main bioactives in PLE targeting bronchitis. PLE and its five bioactive compounds were assessed for their potential anti-inflammatory activities in lipopolysaccharide (LPS)-stimulated RAW264.7 cells. Western blot analysis was conducted to elucidate the associated molecular mechanisms. ResultsThirty-seven compounds in PLE were identified, and twelve main compounds were further quantified in PLE using UPLC-MS/MS. PLE oral gavage administrations (0.6 and 0.12 mg/kg) for 7 days markedly reduced cough frequency, prolonged latency period of cough, reduced phlegm and inflammation in mice. The network pharmacology analysis identified 57 gene targets of PLE against bronchitis. The PI3K/AKT and MAPK signalling pathways were the top two modulated pathways. In RAW264.7 cells, PLE (12.5–50 μg/mL) significantly reduced cyclooxygenase-2 (COX-2), inducible nitric oxide synthase (iNOS), interleukin (IL)-1β, IL-6 and tumor necrosis factor (TNF)-α. PLE downregulated LPS-elevated protein targets in both PI3K/AKT and MAPK signaling pathways. In PLE, tenuifolin, polygalaxanthone ⅠⅠⅠ, polygalasaponin ⅩⅩⅤⅢ, tenuifoliside B, and 3,6′-Disinapoyl sucrose, were identified as the top five core components responsible for treating bronchitis. These compounds were also found to modulate the protein targets in the PI3K/AKT and MAPK signalling pathways. ConclusionsThis study demonstrated the potential therapeutic effects of PLE on bronchitis by reducing cough, phlegm and inflammation. The anti-inflammatory action and molecular mechanisms of the 5 main bioactive compounds in PLE were partly validated through the in vitro assays. The findings provide valuable insights into the mechanisms underlying the traditional use of PLE for bronchitis.

Investigating the etiology of Haff disease: Optimization and validation of a sensitive LC-MS/MS method for palytoxins analysis in directly associated freshwater and marine food samples from Brazil

Haff disease typically develops after eating contaminated marine or freshwater species, especially fish. Despite still having an unknown etiology, recent reports have suggested its possible correlation with palytoxins. Therefore, the present work aimed to optimize and perform a validation of a sensitive method using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) for the analysis of palytoxin and some of its analogs, with the main purpose of investigating their presence in marine and freshwater food samples associated with Haff disease in Brazil. The method optimization was performed using a central composite rotatable design and fish samples fortified with the palytoxin standard. Then, the optimized method was validated for different food matrices, including freshwater and marine fish, mollusks, and crustaceans. The sample preparation involved a solid–liquid extraction using methanol and water, solid-phase extraction using Strata-X cartridges, and on-column palytoxin oxidation. The detection of the main oxidized fragments (amino and amide aldehydes) was achieved by LC-MS/MS with electrospray ionization in positive mode, using a C18 column, as well as acetonitrile and water as mobile phases, both acidified with 0.1 % of formic acid. After optimization and validation, the etiological investigation involved the analysis of 16 Brazilian Haff disease-related food samples (in natura and leftover meals) from 2022. The method was demonstrated to be appropriate for quantitative analysis of freshwater and marine species. So far, it has proven to be one of the most sensitive methods related to palytoxin detection (LOD 10 μg/kg), being able to work in a range that includes the provisional ingestion limit (30 μg/kg). Regarding the Haff disease-related samples analysis, there is a strong indication of palytoxin contamination since the amino aldehyde (common fragment for all palytoxins) was detected in 15 of the 16 samples. Selected results were confirmed using liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS).

Antimicrobial Assessment of Hand Sanitizers Formulated from Neem Leaf Extract (Azadirachta indica) and Coconut Shell Liquid Smoke

Abstract The widespread use of alcohol/ethanol-based hand sanitizers has raised concerns due to the concurrent issues of skin irritation, allergies, childhood poisoning risks, and the potential for bacterial resistance to antibiotics, which may disrupt the human digestive system. This study explores the potential of Neem leaves (Azadirachta indica) and liquid smoke as natural alternatives to alcohol-based antiseptics. The objective is to assess the antimicrobial efficacy of hand sanitizers containing Neem leaf extract and coconut shell liquid smoke against Escherichia coli and Salmonella typhimurium. Hand sanitizers were prepared by mixing 4g of Neem leaf extract with varying quantities of coconut shell liquid smoke (labeled as A1, A2, A3, A4, and A5, corresponding to 0g, 1g, 3g, 5g, and 7g, respectively). distilled water was then added until the total volume reached 100 ml. The solution was then stabilized with 0.5g of Carboxyl Methyl Cellulose (CMC) and 10g of glycerin. Results indicate that formulations A1, A2, A3, and A5 exhibit moderate inhibitory activity against Escherichia coli, with inhibition zone diameters of 6.02 mm, 8.17 mm, 9.67 mm, and 9.11 mm, respectively. Notably, formulation A4 displays strong inhibitory activity (11.15 mm). For Salmonella typhimurium, formulations A4 and A5 demonstrate very strong antimicrobial properties with inhibition zones measuring 11.68 mm and 12.59 mm, respectively. These findings suggest that hand sanitizers comprising Neem leaf extract and liquid smoke possess the potential as environmentally friendly, natural antiseptics.

An updated review of composition, health benefits, and applications of phenolic compounds in Ficus Carica L.

AbstractFicus carica L. (FC) is rich in phenolic compounds such as phenolic acids, flavonoids, and anthocyanins. Phenolic compounds in FC show remarkable health benefits and applications. The composition of phenolic compounds in FC can vary with some factors, such as variety, ripeness, geographical location, extraction methods and processing methods. New techniques such as supercritical fluid extraction, subcritical water extraction and ionic liquid extraction should be further developed and combined with traditional techniques to obtain higher quality sources of phenolic compounds. Numerous in vivo and in vitro studies reported healthy benefits of phenolic compounds in FC, such as anti‐oxidant, anti‐inflammatory, anti‐diabetic, anti‐obesity, anti‐cancer and anti‐Alzheimer's. Further works are required to reveal mechanisms and structure‐activity relationships, such as targeted metabolomics and pharmacological studies. In terms of applications, phenolic compounds in FC as prebiotics on the intestinal flora need to be further studied to expand their applicability in food fermentation. In a word, this review highlights the remarkable health benefits and application value of phenolic compounds in FC.

Research on the Application of Ionic Liquid Extraction Agent in the Enhanced Separation of Allyl Alcohol-Water Azeotropic System

Research on the Application of Ionic Liquid Extraction Agent in the Enhanced Separation of Allyl Alcohol-Water Azeotropic System

Efficacy of Seaweed Liquid Extract from Ulva spp. in Improving Growth and Chlorophyll-a Content of Eucheuma denticulatum in Tissue Culture

Efficacy of Seaweed Liquid Extract from Ulva spp. in Improving Growth and Chlorophyll-a Content of Eucheuma denticulatum in Tissue Culture

Determination of six short‐chain fatty acids in rat feces using headspace solid‐phase dynamic extraction coupled with GC‐MS

Short‐chain fatty acids (SCFAs) are organic acids with carbon atoms less than six, released through fermentation products by intestinal microbiome, having multiple physiological activities. Considering weak acidity and high volatility, derivatization or liquid–liquid extraction is essential, which is time consuming. Headspace‐solid‐phase dynamic extraction (HS‐SPDE) coupled with gas chromatography‐mass spectrometry is automated and effortless to determine SCFAs in rat feces. The extraction procedure is performed by aspirating and discharging the headspace cyclically through a steel needle, coated with an inner polyethylene glycol sorbent. The key parameters of SPDE were optimized including coating type, incubation time and temperature, and number of extraction strokes. Besides, salting‐out was conducted. Then, a method by HS‐SPDE‐GC‐MS was established and validated. It only took 3‐min incubation time, 4.5 min extraction time, and 13 min chromatographic separation in a run. The recovery, linearity, limit of quantification, and stability were evaluated. Then, the proposed method was applied to analyze rat feces including 18 rats with liver injury and 23 normal controls. Mann–Whitney U test indicated that the concentrations of six SCFAs in normal rat feces were higher than those with liver injury. This method provides a choice for fast, solvent‐free, automated, and high‐throughput analysis of SCFAs.

Himatanthus bracteatus stem bark ethanolic extract obtained by sequential pressurized liquid extraction: Chromatographic characterization and profiling of cytotoxic, antitumoral and immunopharmacological properties

This study aims to characterize the cytotoxic, antitumoral and immunopharmacological profile of the ethanolic extract of Himatanthus bracteatus (EEHB) stem bark. Chromatographic analysis revealed the major EEHB composition in dimethyl isoplumerideo acid, 13-deoxyplumerido, isoplumeride, and plumeride. Cytotoxicity was performed on MCF-7 and MCF-10A cell lines using MTT assay. The antitumor activity was assessed using sarcoma 180 tumor cells subcutaneously implanted in mice. After seven days, hematological and biochemical analysis, and pathological evaluation of tumors and visceral organs were carried out. The IC50 value was 28.49 ± 2.05 μg/mL on MCF7 cells, but over 320 μg/mL on MCF-10A cells. Molecular docking was predicted using the caspase 3 molecular target with plumeride and isoplumeride ligands. Both compounds were also analyzed by PreADMET. The tumor growth inhibition was comparable to 5-FU. EEHB reduced the proliferative index (Ki67 immunoexpression) but increased the expression of apoptotic markers in a sarcoma 180 model. The ligands showed interaction with Caspase 3 with a binding energy between −7.2 and −6.6 kcal/mol for isoplumeride and −7.8 to −7.0 kcal/mol for plumeride. Hydrogen interactions were present between the ligands and caspase 3. Both phytochemicals showed low or no permeability in blood-brain barrier and medium permeability in Caco-2 cells and only isoplumeride showed mutagenic potential and carcinogenic. EEHB presented no toxicological effect either on the hematological parameters or average weight and histological features of liver, kidneys, and spleen. Our data suggest that EEHB has antitumor activity in S-180 tumor-bearing mice by blocking cell cycle and increasing apoptosis.

PENGARUH ANTIBAKTERI SEDIAAN SABUN WAJAH CAIR EKSTRAK ETANOL DAUN BELIMBING WULUH (Averrhoa bilimbi L) TERHADAP Staphylococcus aureus METODE DIFUSI

Facial soap used to clean the face from exposure to dust, pollution, dirt, reduce sebum on the face and eradicate bacteria that can cause acne. Star fruit leaves are efficacious in healing several diseases, such as purulent skin inflammation, boils and medicine for gout. Phytochemical of star fruit leaves contain alkaloid, flavonoid, saponin, tannin and steroid compounds that can inhibit bacterial growth. This study aims to determine the effect of liquid facial soap containing of star fruit leaf extract (Averrhoa bilimbi L) on the growth of Staphylococcus aureus bacteria by diffusion method.This study used a Quasi Experiment research design. The population in this study were wuluh star fruit leaves. The sample used is star fruit leaf extract which is made into liquid facial soap preparations with concentrations of 5%, 10%, 15% and 20%. This antibacterial testing method uses the Kirby-Bauer diffusion method. The results of antibacterial research obtained the average diameter of the inhibition zone at 5% concentration of 10.60 mm, 10% concentration of 11.20 mm, 15% concentration of 12.10 mm, and 20% concentration of 13.23 mm. Based on the diameter of the inhibition zone formed at concentration of 5% is categorized as a moderate response and at concentration of 10%, 15% and 20% is categorized as a strong response.The results of simple linear regression statistical analysis obtained p value = 0.000 &lt; α 0.05 which means Ha is accepted, which means that there is a significant effect on the preparation liquid facial soap ethanol extract of star fruit leaves (Averrhoa bilimbi L) against the growth of Staphylococcus aureus diffusion method.

Bio-synthesis, purification and structural analysis of Cyclosporine-A produced by Tolypocladium inflatum with valorization of agro-industrial wastes

Cyclosporine A (CyA) holds significant importance as a strategic immunosuppressive drug for organ transplant patients. In this study, we aimed to produce pure and cost-effective Cyclosporine A (CyA) by fermenting a culture medium containing dairy sludge, using Tolypocladium inflatum PTCC 5253. Following the fermentation stage, ethyl acetate extraction and fast protein liquid chromatography were employed for sample purification. The initial evaluation of the effectiveness of CyA obtained from these processes was performed through bioassay, wherein the antimicrobial clear zone diameter was found to be larger compared to the sample obtained from the fermentation culture. The concentration of CyA was determined using high-performance liquid chromatography, yielding values of 334 mg/L, 456 mg/L, and 578 mg/L for the fermented, extracted, and purified samples, respectively. Further analysis utilizing liquid chromatography tandem mass spectrometry (LC/MS/MS) confirmed a purity of 91.9% and proper agreement with the standard sample based on the ion intensity of Z/m 1205. To validate the structure of CyA, nuclear magnetic resonance spectroscopy, Fourier-transform infrared (FT-IR), and Raman spectroscopy were employed. X-ray diffraction and differential scanning calorimetry analyses demonstrated that the purified CyA exhibited a crystal structure similar to the standard sample, characterized by two broad peaks at 2θ = 9° and 20°, and comparable glass transition temperatures (57–68 °C for the purified sample; 53–64 °C for the standard sample). Dynamic light scattering analysis confirmed a uniform particle size distribution in both the purified and standard samples. The zeta potentials of the purified and standard samples were determined to be − 25.8 ± 0.16 and − 23.63 ± 0.12 mV, respectively. Our results demonstrate that dairy sludge can serve as a suitable culture medium for the production of (CyA).

Radiation resistant metal–organic frameworks for the production of high specific activity 51Cr by the Szilard-Chalmers effect

Chromium-51 (51Cr) is an attractive radionuclide for diagnosis, which is usually applied for red cells and platelet radiolabeling. However, commercially available 51Cr produced in nuclear reactors via neutron activation requires long irradiation times and complex separation methods. In this work, five metal–organic frameworks (MIL-100 (Cr), MIL-100 (Fe), MIL-100 (Al), MIL-101 (Cr) and aluminium fumarate MOF (FuAl)) were synthesized and the effect of gamma ray irradiation with a high dose rate and a maximum dose of 6 MGy was investigated. The two chromium-based MOFs, MIL-100 (Cr) and MIL-101 (Cr), were selected as radiation targets to produce high specific activity 51Cr by the Szilard-Chalmers effect. A solid–liquid extraction was applied to extract the produced 51Cr under different conditions, including different extractants, extraction times and pH. The most promising results were achieved when using irradiated MIL-101 (Cr) and EDTA as extracting agent, reaching an enrichment factor of 1132 ± 50.

Application of newly developed and validated LC-MS/MS method for pharmacokinetic study of adagrasib and pembrolizumab simultaneously in rat plasma

Non-small cell lung cancer (NSCLC) is a significant subtype of lung cancer, and poses a dangerous global threat. One of the current approaches of NSCLC treatment is a combination therapy of adagrasib and pembrolizumab. Accurate monitoring of these drug concentrations in biological fluids is critical for treatment efficacy. Since no method was reported for simultaneous estimation of these drugs, this study focuses on the development of a validated LC-MS/MS bioanalytical method for simultaneous quantification of Adagrasib and Pembrolizumab in rat plasma. The analytes were extracted from the biological matrix through liquid–liquid extraction techniques using acetonitrile as extraction solvent. The analytes were separated on a Waters X-bridge phenyl C18 column, with a mixture of acetonitrile: 0.1 % TFA in water (50: 50 v/v) as mobile phase at an isocratic flow rate of 1.0 mL/min with a runtime of about 5 min. Adagrasib (m/z 605.12 → 201.62), Pembrolizumab (m/z 146.32 → 85.15), and Sotorasib (m/z 561.59 → 218.92) were determined by recording the mass spectra through multiple reaction monitoring in positive mode. The method was validated according to USFDA guidelines. The results demonstrate satisfactory linearity with an r2 value of 0.9998 in the ranges of 40–800 and 10–200 ng/mL, accuracy with mean percentage recovery of 95.22–98.59 % and 96.98–98.57 %, precision indicated with %RSD ranged between 0.39–1.91 % and 0.85–9.03 % for Adagrasib and Pembrolizumab respectively, and other key parameters. The developed method can determine the pharmacokinetic parameters to indicate the efficacy and safety of the drugs, and also can quantify selected drugs simultaneously in biological samples.