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Chemical engineering is an engineering branch that deals with the chemical production and manufacture of products that undergo chemical processes. This includes equipment design, creating systems and processes to refine raw material, as well as mixing, compounding, and processing chemicals to create products.
Chemistry and Chemical Engineering
Abstract
The first targeted Rho-associated protein kinase 2 inhibitor was Belumosudil (Rezurock). After at least two systemic treatments failed for chronic graft-versus-host disease in adults and children aged 12 and older, belumosudil (BLS) was approved on July 16, 2021. This study established a validated Ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) system to estimate BLS in HLMs and assess metabolic stability. Agilent C18 column was used to separate BLS and encorafenib (internal standard) in HLMs using an isocratic mobile phase. The electrospray ionization (ESI) source produced BLS parent ions. Multiple reaction monitoring identified and measured BLS daughter ions. The methodology was validated following FDA standards that assessed linearity, selectivity, accuracy, sensitivity, precision, extraction recovery, matrix effects, and stability. The accuracy and precision ranged from −1.42 to 12.50% between days and from −0.89 to 10.5% within a day. The created BLS calibration curve displayed a linearity in the range from 1 ng mL−1 to 3,000 ng mL−1. The LLOQ of 0.64 ng mL−1 showed the method's sensitivity. The AGEE program displayed that the approach was eco-friendly. In vitro half-life and intrinsic clearance of BLS were 17.55 min and 46.21 mL min−1 kg−1, demonstrating a high extraction ratio drug. These features can improve the metabolic stability of new derivatives compared to BLS, making them important in medication design.
Abstract
The magnitude of the interactions between two phases may be deduced from results collected by various experimental techniques. One of them is Inverse Gas Chromatography (IGC).
The aim of the work was to compose and examine various polymer blends of PVC/PMMA, PMMA/PS and PVC/PS. Behavior of these blends was characterized by using the Flory-Huggins parameters estimated by means of the IGC. Based on the obtained results, the miscibility of the components in the tested polymer blends was determined. Characteristics derived from IGC data were compared with literature data calculated from equilibrium solvent (methanol) absorption.
Abstract
In this study, a simple, fast, and sensitive stability indicating CE method was developed for the quantification of Triamterene (TRM) and Hydrochlorothiazide (HCT) in pharmaceutical preparations. Detection was achieved using a photo diode array detector, and the separation process was conducted in a capillary with an inner diameter of 75 µm and a length of 40 cm. Optimum conditions were achieved by using a run buffer of 15 mM borate containing 20 mM SDS at pH 9.00, and applying a potential of 25 kV. HCT and TRM exhibited migration times of approximately 2.75 ± 0.007 min and 4.61 ± 0.022 min, respectively, under these conditions. The developed method was validated by assessing parameters such as linearity, selectivity, precision, accuracy, sensitivity, stability, and robustness. To assess the selectivity of the method, HCT, TRM, and tablets containing these compounds were exposed to acidic, basic, oxidative, thermal, and photolytic stress conditions. Ultimately, the method was proved successfully in accurately determining HCT and TRM levels in tablets.
Abstract
This study examined the effect of grapefruit seed extract (GSE) (0%–3%) on the stability of total phenolic content (TPC), anthocyanins, and colour in aronia juice under heat treatments (60 °C, 80 °C for up to 120 min). TPC and anthocyanins were measured using spectrophotometry and HPLC. The highest TPC (8545.02 ± 355.55 GAE mg L−1) was measured in aronia juice with 1% GSE after 60 min at 80 °C. The highest anthocyanin retention (3178.75 mg L−1) was detected in the sample with 1% GSE after 5 min at 60 °C. Cyanidin-3-galactoside was the most abundant anthocyanin, followed by cyanidin-3-xyloside and cyanidin-3-arabinoside. Cyanidin-3-arabinoside showed the lowest heat stability, while cyanidin-3-galactoside was relatively more stable. This study, the first to evaluate anthocyanin half-life values in chokeberry juice, suggests that 1% GSE enhances colour stability during heat treatment, supporting its use as a natural food additive.
Abstract
ASP3026 is a recently formulated and highly selective inhibitor designed to target the ALK kinase. ASP3026 efficiently inhibited ALK kinase activity and demonstrated superior selectivity at a panel of Tyr-kinases compared to crizotinib. The target of this investigation was to establish a highly accurate, fast, green, and highly sensitive Ultra-high performance liquid chromatography- Tandem mass spectrometry (UHPLC-MS/MS) technique for assessing the concentration of ASP3026 in human liver microsomes (HLMs). In vitro incubation, the metabolic stability of ASP3026 in HLMs was evaluated using this known approach. The validation steps for the UHPLC-MS/MS analytical technique in the HLMs were performed along with the bio-analytical method validation guidelines settled by the US-FDA. To increase the ecological sustainability of the current UHPLC-MS/MS system, a lower flow rate of 0.3 mL min−1, a shorter elution duration of 1 min, and a reduced consumption of ACN have been implemented. A screening of the chemical structure of ASP3026 for hazardous alerts and metabolic lability was performed by the StarDrop package, that includes the DEREK and P450 modules. The analytical separation of ASP3026 and fenebrutinib (FNB) on the reversed phase Eclipse Plus C18 column was performed using an isocratic mobile phase approach. The calibration curve produced by the ASP3026 showed a linear association over the level range of 1–3,000 ng mL−1. A study was conducted to evaluate the precision and accuracy of UHPLC-MS/MS technology in evaluating both intra-day and inter-day variations. The accuracy exhibited a range of −1.56%–7.33% across various days, and a range of −0.78%–10.66% within the same day. The ASP3026 underwent in vitro half-life and intrinsic clearance measurements, yielding values of 14.32 min and 56.62 mL min−1 kg−1, correspondingly. According to in silico software research, using minor modifications to the piperazine component or substituting the group in drug design has the potential to improve the metabolic safety and stability of novel derivatives in comparison to ASP3026.
Abstract
In this experiment, ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was employed to quantify karacoline in mouse plasma following both intravenous and oral administration, thereby elucidating the pharmacokinetic characteristics of karacoline in mice. The analytes were extracted from mouse plasma using acetonitrile for protein precipitation. Chromatographic separation was performed on an HSS T3 column via gradient elution, with the mobile phase consisting of methanol and 0.1% formic acid in water. Quantification of karacoline and the internal standard (IS) was achieved using multiple reaction monitoring (MRM) mode. Six mice received an intravenous (i.v.) injection of karacoline at a dose of 1 mg kg−1, while another six mice were administered karacoline orally (p.o.) at a dose of 5 mg kg−1. The calibration curve for karacoline in mouse plasma ranged from 1 ng mL−1 to 2,500 ng mL−1. The intra-day precision was within 10.4%, and the inter-day precision was within 13.0%. Accuracy ranged from 89.1% to 107.5%, with recovery rates between 77.6% and 88.2%. Matrix effects were observed within the range of 77.6%–107.4%. This method successfully estimated the pharmacokinetics of karacoline, and its bioavailability was determined to be 27.2%, these are preliminary studies that require verification on a larger group of animals.
Abstract
An alternative to roller mills, a French-designed stone mill, was evaluated and compared with traditional laboratory roller mills through grinding performance. Developed by the Astrié brothers in the 1950s, the stone mill's slow-rotating granite stones purportedly preserve the full nutritional value of the grain. This study, conducted in collaboration with the Csoroszlya farm, compared flour from the same wheat batch ground by both an Astrié stone mill and a laboratory roller mill. Evaluations included the Pekar test for bran content, sieve analysis, measuring wet gluten content, and gluten index to assess protein quality. Rheological properties of the doughs were analyzed using Farinograph and Mixolab equipment, which indirectly also measured amylase enzyme activity. Results indicated that the stone mill produced flour with finer grain size, higher protein content, and higher enzyme presence, although challenges remain in achieving optimal gluten index and dough stability.
Abstract
In this study, a simple, rapid, and sensitive capillary electrophoresis (CE) method was developed that allows simultaneous analysis of zonisamide (ZNS), rufinamide (RFN), and lamotrigine (LMT) in pharmaceutical preparations. This study introduces the first application of CE for the simultaneous determination of ZNS, RFN, and LMT in pharmaceutical dosage forms. For the comparison a High-Performance Liquid Chromatography (HPLC) method was developed. In CE method, detection was achieved using a photodiode array detector (DAD) at a wavelength of 210 nm. A capillary with an internal diameter of 75 µm and an effective length of 40 cm was used for separation. The optimum conditions were achieved using 35 mM SDS, 6 mM borate, 10 mM phosphate buffer (pH 9.00) containing 5% isopropyl alcohol (IPA), and applying a potential of 15 kV. Under these conditions, the migration times of ZNS, RFN and LMT were observed to be 5.99 min, 6.77 min and 8.46 min, respectively. In HPLC method, detection was achieved using a photodiode array detector at a wavelength of 210 nm. A C18 column (4.6 × 100.0 mm, 3.5 µm i.d.) was used for separation, with a mobile phase consisting of acetonitrile and pH 4.0 50 mM phosphate buffer (18:82, v/v) at a flow rate of 1.0 mL min−1. In this method, the retention times of ZNS, RFN and LMT were observed to be 6.41 min, 7.29 min and 4.95 min, respectively. The validity of the developed methods was examined through parameters such as linearity, precision, accuracy, sensitivity, stability, and robustness. In CE method, the limit of detection (LOD) values for ZNS, RFN and LMT were calculated as 0.035 μg mL−1, 0.016 μg mL−1 and 0.007 μg mL−1, respectively. For HPLC method, the LOD values were determined as 0.003 μg mL−1, 0.002 μg mL−1 for RFN and 0.001 μg mL−1 for LMT. Both developed methods were successfully applied to pharmaceutical dosage forms and shown to be compliant with United States Pharmacopeia (USP 47 - NF 42). In conclusion, both methods developed in our study yielded comparable results in terms of robustness and analysis time. HPLC demonstrated higher sensitivity compared to CE and is preferred for analyses at very low concentrations, while CE is ideal for green chemistry applications due to its minimal solvent and sample consumption.
Abstract
Violanthin, a compound isolated from the stems of Dendrobium officinale, exhibits potent antioxidant and antibacterial activities. However, no research has been conducted on the identification of violanthin in mouse plasma using UPLC-MS/MS. The present study aims to develop a selective UPLC-MS/MS method for the quantification of violanthin in mouse plasma. Samples were prepared using acetonitrile for protein precipitation, with aconitine as an internal standard (IS). Chromatographic separation was achieved on a UPLC HSS T3 column with acetonitrile and 0.1% formic acid as the mobile phase. Quantification was performed in multiple reactions monitoring (MRM) mode, targeting fragment ions m/z 579.6→457.2 for violanthin and m/z 646.6→586.5 for IS. Mouse blood samples were collected at different time points following intravenous (4 mg kg−1) and oral (30 mg kg−1) administration of violanthin. The calibration plots for violanthin in mouse plasma exhibited a linear trend across the entire range of 5–2,000 ng mL−1, with both intra-day and inter-day precision RSDs below 10%. The bioavailability was determined to be 24.3%. This UPLC-MS/MS method effectively facilitated pharmacokinetic studies of violanthin in mice.
Abstract
The determination of total flavonoid content (TFC) through the aluminum chloride (AlCl3) colorimetric test utilizing spectrophotometry is commonly used as a parameter for evaluating the quality of processes as well as food and herbal medicines materials. Nonetheless, it is laborious, lengthy, and necessitates substantial amounts of chemicals. This study aims to develop and validate the dot-blot assay with AlCl3 reagent for determining TFC in plant materials. In this method, the samples were not subjected to chromatography; instead, the plates were derivatized using AlCl3 in ethanol immediately after the application of samples and evaporation the solvent. The Al(III)-flavonoid complex was scanned (421 nm) using a TLC-scanner. The validation of the method was conducted on stability, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The TFC of samples determined by dot-blot assay and spectrophotometry was subsequently analyzed using linear regression and Pearson correlation. The dot-blot assay for determining TFC met the stability parameter (RSD = 1.31–8.25%), intraday precision (RSD = 2.20–6.11%), inter day precision (RSD = 1.56%), linearity (r 2 = 0.9928), LOD (251.03 ng/spot), LOQ (760.71 ng/spot), accuracy (recovery = 70.81–75.61%), and robustness (RSD = 2.55 and 7.60%). There was a very strong positive linear relationship between the dot-blot assay method and spectrophotometry, with a linear regression coefficient of 0.9078 and a Pearson correlation coefficient of 0.911. The proposed method proved to be simpler, faster, and more economical for determining TFC. Thus, the method was beneficial in providing references for enhancing the quality control of food and herbal medicines.
Abstract
We developed and validated a liquid chromatography–mass spectrometry (LC–MS/MS) method for detecting conivaptan, an arginine vasopressin receptor blocker, in human plasma to facilitate future pharmacokinetic studies. After acetonitrile protein precipitation, analytes were separated on a Grace Alltima HP C18 reverse-phase column (5 μm, 2.1 × 50 mm), and gradient elution was performed using 0.1% formic acid and 5 mM ammonium formate in acetonitrile–water (1:9) and acetonitrile–water (9:1) over a 4-min run time. Positive-mode electrospray ionization and multiple reaction monitoring were applied. The assay was linear over the concentration range of 1–500 ng mL−1, with confirmed accuracy (intra-batch, 0.5–1.1%) and precision (intra-batch relative standard deviation [RSD], ≤5.7%; inter-batch RSD, ≤6.8%). Extraction recovery varied between 94.2–100.5%, and the matrix effect was 94.9–97.0%. To establish the stability, we examined plasma for 17 h at room temperature, 21 h at 2–8 °C, 57 days at −70 °C for three freeze-thaw cycles, and after processing for 52 h in the autosampler. We detected acceptable stability under all examined conditions. Hemolysis, hyperlipidemia, and dilution integrity satisfied the validation criteria. The method developed in this current study will help accurately quantify conivaptan in human plasma and define its clinical pharmacokinetics in the future.
Abstract
This work developed and validated a new UV-HPLC method for the separation and quantification of vonoprazan fumarate (VNP), amoxicillin (AMX), and clarithromycin (CLM), together in a ternary mixture and in laboratory-prepared tablets. A C18 column and a delightful 70:30 blend of 0.05 M KH2PO4 buffer pH 6 and acetonitrile were used as mobile phase. The flow rate was 1.5 mL min−1, while the wavelength of detection was 254 nm. Linear concentration ranges of (1.0–10.0 μg mL−1) vonoprazan fumarate, (1.0–125.0 μg mL−1) amoxicillin, and (25.0–1,200 μg mL−1) clarithromycin resulted in 0.061, 0.6213, and 7.302 μg mL−1 detection levels and 0.1849, 0.845, and 22.127 μg mL−1 quantification values for VNP, AMX, and CLM, respectively. The greenness of this method was evaluated using the National Environmental Methods Index assessment (NEMI), analytical Eco-scale Assessment (ESA) tool, Green Analytical Procedure Index assessment (GAPI), and Analytical Greenness metric assessment (AGREE), which authenticated the method to be eco-friendly. This method, which was systematically validated and used also to calculate the concentration of the three drugs in their dosage forms, showed high accuracy and precision. Additionally, it produced peaks that were clearly separated and resolved, demonstrating its robustness and specificity.
Soil organic carbon (SOC) levels directly affect the production and health of crops. Making use of a database of the usefulness of using the 350–2,500 nm Near Infra Red (NIR) spectroscopy data range on 200 soil samples from the Indian state of Uttar Pradesh was evaluated in this study. The more sophisticated Artificial Neural Network, to choose the spectral components that were used to forecast SOC, Random Forest (RF) and Ensemble Lasso-Ridge Regression (ELRR) were utilized. In the preprocessing, the inversion derivative, logarithmic(log) derivative, and logarithmic base to 10(log10x) derivatives were employed to duplicate the spectrum wavelength. The main characteristic of spectrum wavelength for SOC were found to be within the range of 350 and 450 nm, per the results. The best accurate estimation of SOC content was obtained by combining the suggested DSANN or Dropout Sequential ANN technique with the Log10x pre-processed data. The R-squared (R2), RMSE, and RPIQ (Ratio of Performance in Inter Quartile Distance) values for the testing dataset were 0.83, 0.08, and 4.32, respectively.
Abstract
The preservation of water resources is seriously threatened by the rise of pharmaceutical contamination. Ribavirin, a widely used antiviral drug, is among the pharmaceutical residues in wastewater. In this study, the adsorption capacity of activated carbon produced from tobacco stems, a by-product of the cigarette industry, was investigated. The produced activated carbon was characterised by BET, SEM-EDX and FTIR analyses. In the next step, removal of ribavirin from aqueous solutions using activated carbon was investigated. In the next step, the removal of ribavirin from aqueous solutions was tested with this activated carbon. Various factors such as initial ribavirin concentration (10–50 μg mL−1), solution pH (4–10), adsorbent amount (5–30 mg per 50 mL solution), contact time (0–150 min) and temperature (300–328 K) were investigated to determine the optimum adsorption conditions. Adsorption kinetics were investigated with first and second order pseudo models, and the equilibrium state was analyzed with Langmuir and Freundlich isotherm models. Thermodynamic parameters were calculated at different temperatures (300, 308, 318 and 328 K). The results show that a maximum removal efficiency of 91.83% was achieved at an initial concentration of 30 μg mL−1, adsorbent dose of 20 mg, contact time of 90 min and pH 7.00. The adsorption process was best described by the pseudo-second order kinetic model (R 2: 0.9987) and Langmuir isotherm model (R 2: 0.9971). Thermodynamic analysis shows that the process is spontaneous (ΔG < 0), exothermic (ΔH < 0) and causes a decrease in disorder in the system (ΔS < 0). This study reveals that tobacco stems can offer an environmentally friendly and economic treatment alternative.
Abstract
Aflatoxins (AFs) and deoxynivalenol (DON), common mycotoxins in cereals, pose contamination risks in beer production, often persisting from raw barley into final products. This study investigates the transfer and decomposition of AFs and DON during the barley steeping stage of malting. Barley spiked with AFs and DON was steeped, and mycotoxin concentrations were analyzed in both the barley residue and the resulting wastewater. Results indicated that AF and DON transfer into wastewater was influenced by water solubility, though concentrations remained below solubility limits. AFs and DON residues were also detected in the steeped barley. Decomposition studies showed that while AFs were partially degraded by UV light, DON required photocatalysis for effective degradation. However, matrix components in wastewater decreased the efficiency of DON decomposition, suggesting that preliminary removal of organic components from wastewater could enhance photocatalytic detoxification. These findings provide insight into mycotoxin management strategies for brewing wastewater, emphasizing the need for targeted pretreatment to improve degradation efficiency.
Abstract
The aim of the current investigation to estimate the amount of theobromine (THEOB), theophylline (THEOP) and caffeine (CAF) concurrently using ultra performance liquid chromatography with photo diode array detector (UPLC-PDA) in ultrasound assisted extract of commercially available food products. The commercially available products are categorized in three different groups including teas, coffees and chocolates. The UPLC approach is rapid, precise, highly sensitive and cost effective for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. The mobile phase comprises a mixture of water and ACN (90:10, v/v) for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. The current approach operated on a linear scale range of 6.66–33.3 ng mL−1, 3.33–33.3 ng mL−1 and 3.33 – 33.3 ng mL−1, respectively, for THEOB, THEOP and CAF at 272.5 nm wavelength. The LOD for THEOB, THEOP and CAF were assessed to be 1.10 ± 0.001, 0.75 ± 0.000 and 0.48 ± 0.002 ng mL−1, respectively by applying the present approach. The LOQ for THEOB, THEOP and CAF were assessed to be 3.35 ± 0.009, 2.29 ± 0.001 and 1.47 ± 0.001 ng mL−1, respectively by applying the present approach. These findings confirmed that the current UPLC approach is highly sensitive, accurate, precise and robust for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. Antioxidant activity of different teas, coffees, chocolates as well as standard THEOB, THEO and CAF were determined by DPPH method.
Abstract
Osimertinib (Tagrisso, AstraZeneca Pharmaceuticals) is the inaugural third-generation irreversible EGFR-TKI that specifically targets both the EGFR T790M resistant mutation and EGFR-TKI-sensitizing mutations. On September 25, 2024, the Food and Drug Administration authorized osimertinib (OSM) for adult patients with locally advanced, unresectable (stage III) non-small cell lung cancer (NSCLC). The target of this work was to establish a fast, accurate, environmentally friendly, and highly sensitive UPLC-MS/MS methodology for detecting OSM levels in human liver microsomes (HLMs). The separation of OSM and zanubrutinib (ZNB) was accomplished utilizing a C8 column and an isocratic mobile phase. The linearity of the OSM calibration curve spanned from 1 to 3,000 ng mL−1. The AGREE score of 0.76 validates the efficacy of the current approach. The brief in vitro half-life (23.72 min) and moderate intrinsic clearance (34.18 mL min−1 kg−1) of OSM indicate that it resembles drugs with a moderate extraction ratio. The present LC-MS/MS technique is regarded as the primary analytical methodology for quantifying OSM in HLM matrices. The characterization of OSM metabolic stability and in silico ADME features are crucial for progressing the discovery of novel drugs with improved metabolic stability.
Abstract
Apples are among the most common fruits, produced on the territory of North Macedonia. Before they reach the market, it is essential to be tested for pesticide residues, which are used for protection against pests for this culture, and in order to ensure the customer safety. For this reason, a novel and simple method for simultaneous determination of captan, folpet, difenoconazole and chlorpyrifos in apple samples has been developed and validated. Acetone is used for extraction of the pesticide residues, followed by liquid-liquid (LLE) and solid–phase extraction (SPE). Separation and quantification of analytes is achieved on reversed-phase high performance liquid chromatography (RP-HPLC) with UV diode array detector (UV-DAD). The best results are obtained using analytical column LiChrospher 60 RP-select B (250 mm × 4 mm, 5 µm), with isocratic elution and acetonitrile/0.1 % acetic acid in water (70:30, V/V) as a mobile phase. The flow rate is 1 mL min−1, and UV detection is performed at 220 and 230 nm. The linearity of the method is tested in the range of 1.50–3.60 mg kg−1 for captan and folpet, and 0.35 – 0.60 mg kg−1 for difenoconazole and chlorpyrifos. The obtained values for recovery and RSD ranged from 94.94 to 114.63 %, and 0.09–9.25 %, respectively. The validated method is successfully applied to apple samples for the determination of the investigated pesticide residues.
Abstract
Aflatoxins, potent carcinogenic mycotoxins produced by Aspergillus species, persist in various foods, posing significant health risks upon consumption. This study assesses dietary aflatoxin B1 (AFB1) exposure in Vietnam using Margin of Exposure (MOE) and Hazard Index (HI) to evaluate risk levels in peanuts, chili powder, corn, and raisins. AFB1 levels were quantified by UPLC-FLD. AFB1 was detected in 71.5% of chili powder, 29.3% of peanuts, and 26.0% of corn samples, with no detectable levels in raisins. Peanuts and corn kernels were classified as high-risk, with MOE values below 10,000 (peanuts: 25.8–56.6; corn: 42.3–92.6) and HI values exceeding 1, potentially contributing to 20.4–44.7 and 12.5–27.3 liver cancer cases per 100,000 adults, respectively. In contrast, chili powder had MOE values between 3,208 and 7,021 and HI below 1, indicating a low public health risk. Raisins were deemed safe with MOE over 200,000 and HI at 0.01. Results also indicated higher cancer risk for women and lean individuals consuming the same AFB1 levels. These findings underscore the need for focused risk management strategies to mitigate AFB1 exposure and protect public health in Vietnam.
Abstract
In the field of pharmaceutical analysis, high-performance liquid chromatography (HPLC) is considered to be the key technique, which is one of the most efficient, quick, and easy methods for the simultaneous determination of two are more drugs. The purpose of the current study is to develop and validate the reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of Paracetamol and Fexofenadine HCl. This approach was validated by the standards and The International Conference on Harmonization (ICH), and United States Pharmacopeia (USP) were followed in the development and validation of the method. The chromatographic conditions including a mobile phase comprised of a 35:65 buffer mix and acetonitrile with a 1.0 mL min−1 flow rate were used. A thorough investigation was performed, including linearity and range, specificity, robustness, accuracy, precision, solution stability, and system suitability. The outcomes of the studies have shown that, both Active Pharmaceutical ingredients i.e., Paracetamol and Fexofenadine HCl were separated in about 7.5 min. The variation coefficient for Paracetamol and fexofenadine HCl varied between 0.9992 R 2 and 0.9983 R 2, respectively. The devised method was proved accurate, as API recoveries in both cases of Paracetamol and Fexofenadine ranged from (99.79%, 100.72%, and 98.64%) to (99.96%, 100.64%, and 99.00%). The method's accuracy was further demonstrated by the solution stability which was 99.84% for Paracetamol, and 100.53% for Fexofenadine HCl. The suggested method for simultaneously measuring Paracetamol and Fexofenadine HCl was established, validated, and there was no evidence of any excipient interaction was observed.
Abstract
The need to develop environmentally friendly analytical approaches has driven the pharmaceutical industry to seek greener alternatives. Ultra-Performance Liquid Chromatography (UPLC) is known for its efficiency but traditionally relies on toxic solvents. Integrating Green Analytical Chemistry (GAC) principles aims to address environmental concerns while maintaining analytical performance. This work aims to advance and authenticate a green, efficient UPLC method for the concurrent quantification of Metformin (MET) and Empagliflozin (EPI) in tablet formulations, adhering to green chemistry principles and ensuring high analytical accuracy. The method was optimized using a UPLC-PDA system with a phenyl column and a mobile phase of ethanol and perchloric acid. Analytical Quality by Design (AQbD) was employed to optimize critical method parameters. Environmental impact was assessed using metrics such as GAPI, AMGS, and AGREE. Degradation studies under various stress conditions were performed to test method robustness. The method achieved high recovery rates for MET and EPI, with minimal interference from excipients. The environmental evaluation showed a high Analytical Eco-Score (AES) of 97, indicating low environmental impact. The AGREE score of 0.89 confirmed excellent alignment with green chemistry principles. Degradation studies confirmed the method's stability and reliability under stress conditions. The developed UPLC method demonstrates a significant advancement in analytical sustainability, offering an eco-friendly, efficient, and precise approach to drug analysis. The method's high alignment with green chemistry principles and its effectiveness in quantifying MET and EPI highlight its potential as a model for sustainable analytical practices in pharmaceutical analysis.
Abstract
Tea's beneficial effects have long been attributed to its abundance of natural bioactive compounds; however, the influence of variations in these compounds on taste and aroma remains poorly understood. To investigate the relationship between metabolomic profiles and tea processing adaptability, this study employed sensory evaluation and untargeted metabolomics to compare four tea cultivars from Guangxi—Ying Hong No.9 (YH), Gui Hong No.3 (GH), Gui Cha No.2 (GC), and Mei Zhan (MZ)—cultivated under the same conditions. Sensory evaluation revealed that GH and MZ exhibited the highest quality in green tea and black tea, respectively, while GC showed moderate quality, and YH performed less favorably than the other three cultivars. Metabolomics analysis uncovered significant differences in the metabolic profiles among the four tea cultivars, with MZ and YH displaying higher levels of flavonol glycosides, and GC and GH showing elevated levels of organic acids and fatty acids. Pathway analyses of GH and MZ indicated that the differentially enriched pathways were primarily related to linoleic acid metabolism and flavonoid and flavanol synthesis. Correlation analyses further revealed that the sensory quality of green tea was closely linked to fatty acids and organic acids in fresh leaves, whereas the sensory quality of black tea was strongly associated with flavonol glycoside levels. This study provides a comprehensive understanding of the complex relationship between metabolite characteristics and processing suitability in different tea cultivars, offering valuable insights into the development of tea germplasm resources in the Guangxi region.
Abstract
This research dealing with salting out TLC technique for simultaneous determination of two antihistaminic drugs Loratadine and its active metabolite desloratadine in pure, tablets and rabbit spiked plasma. Separation was performed on silica gel 60 F254 plates using aqueous ammonium sulfate and acetonitrile (6:4, v/v) as a mobile phase. The R f values were 0.51 ± 0.02 and 0.70 ± 0.004 for Loratadine and desloratadine, respectively in pure or dosage form while in spiked plasma R f values were 0.39 ± 0.004 and 0.61 ± 0.004 for both drugs respectively using levocetirizine as internal standard (R f 0.74 ± 0.004). The separated bands were scanned under UV light at λ 254 nm and the TLC chromatograms were captured by camera and treated with Image J software. Method validation was according to ICH and complied with USP31- NF26 guidelines. The correlation coefficients of calibration curves were 0.997 and 0.998 for Loratadine and desloratadine in pure and dosage form while in rabbit spiked plasma were 0.996 and 0.995 for both drugs respectively in the range 100–2,000 μg mL−1. limits of detection LOD and limits of quantitation LOQ for Loratadine and desloratadine were 7.84, 30.06 and 23.52, 91.18 μg mL−1 respectively as pure or as dosage form while LOD and LOQ in rabbit spiked plasma were 17.46, 14.03 and 52.38 and 42.09 μg mL−1 respectively.
Abstract
The automated system for enhancing plant growth presents an innovative approach to optimize quality of sugarcane cultivation for four main sugarcane growing zones. It includes issues like recommendation of crops based on soil nutrients, diagnosis of disease in the leaf and stem images of sugarcane, weed detection and harvesting time prediction. The research work proposed in the article presents an innovative two-stage approach for object detection and classification in agricultural imagery. Initially, YOLOv8 (You Only Look Once) is employed to accurately detect objects within images, delineating them with precise boundary boxes. Subsequently, the focus of hybrid model integrating Convolutional Neural Networks (CNNs) and Long Short-Term Memory (LSTM) networks, known as Contextual Long Short-Term Memory (CLSTM), is employed. This dual-stage methodology harnesses the speed and accuracy of YOLOv8 for robust object localization, while the CLSTM model ensures nuanced classification, contributing to comprehensive and accurate approach for object detection and crop-weed differentiation in agricultural scenarios. The proposed approach is compared with the four DL algorithms for identifying weeds in sugarcane crops and subsequently assessed their accuracy and F1 score performance. At a learning rate of 0.002, the findings of CLSTM showcase superior precision at 98.5%, recall at 97.8%, F1 score at 98.1%, and an overall accuracy of 97.7%. The subsequent task is harvesting time prediction, which entails identifying the best time to harvest sugarcane based on the planting period, weather predictions, and sugarcane brix value. The implementation of this automated system not only enhances the productivity of sugarcane cultivation but also serves as a model for sustainable and resource-efficient agriculture.
Abstract
Febrifugine, a potent quinazolinone compound derived from the Chinese herb Chang Shan (Dichroa febrifuga), exhibits diverse biological activities and has demonstrated anti-tumor effects by functioning as focal adhesion kinase (FAK) inhibitors. In this study, our objective was to establish a quantitative UPLC-MS/MS method and investigate the pharmacokinetic characteristics of febrifugine in rats following intravenous and oral administration routes. The rat tail vein was used for the collection of blood samples at designated time intervals following intravenous (2.0 mg kg−1) and oral (6.0 mg kg−1) administrations. Plasma samples were pretreated with acetonitrile as a protein precipitant and methylcytisine as an internal standard. Febrifugine concentration in rat plasma was determined using the UPLC-MS/MS method, and pharmacokinetic parameters were calculated using drug and statistics (DAS) software version for statistical analysis. The linear range of febrifugine in rat plasma was 1.5–1,500 ng mL−1, meeting the precision, recovery, and stability requirements for determination purposes. Febrifugine had a half-life (t1/2) of 3.2 ± 1.6 h after administered via intravenous route, while t1/2 was 2.6 ± 0.5 h after oral administration. The developed UPLC-MS/MS method is facile to operate while adhering to rigorous methodological verification standards, rendering it suitable for investigating the pharmacokinetics of febrifugine; and bioavailability was determined as 45.8%.
Abstract
This study presents the development and validation of a robust HPLC-UV method for the simultaneous detection and quantification of vitamin D2, vitamin D3, ergosterol, and 7-dehydrocholesterol in a single analytical run, adhering to ICH Q2 (R1) guidelines. Application of the HPLC-UV method to six vegetable oils demonstrated inherent vitamin D content and its enhancement under different radiation conditions. Oils were exposed to direct sunlight, UVA, and UVB radiation, with UVB showing the most significant impact on vitamin D levels. Notably, UVB exposure increased vitamin D3 in castor oil from 2.82 μg mL−1 to 4.29 μg mL−1 and vitamin D2 in mustard oil from 0.73 μg mL−1 to 1.89 μg mL−1. The findings highlight the potential of UVB radiation to convert vitamin D precursors to active forms more effectively than other radiation sources. This study provides a novel approach for naturally enriching vitamin D in vegetable oils, offering a promising strategy to mitigate vitamin D deficiencies in populations with limited sun exposure or dietary restrictions. The developed HPLC-UV method and resultant insights into the radiation-induced enhancement of vitamin D content in oils contribute valuable knowledge to nutritional science.
Abstract
Zanubrutinib (Brukinsa, BeiGene) is a FAD approved second-generation Bruton's tyrosine kinase inhibitor that has more selectivity and reduced off-target action, resulting in mitigated cardiotoxicity compared to ibrutinib. The target of this investigation was to establish a fast, precise, green, and extremely sensitive UPLC-MS/MS approach for quantifying the level of zanubrutinib (ZNB) in human liver microsomes (HLMs). The separation of ZMB and revumenib was achieved using C8 column and isocratic gradient of the mobile phase. The linearity of the constructed ZNB calibration curve was ranged from 1 to 3,000 ng mL−1. The StarDrop software package including DEREK and WhichP450 modules was used in screening for the toxic alerts the in silico metabolic lability of ZNB. The AGREE score was 0.76 that approves the greenness of the established method. The low in vitro t1/2 (17.61 min) and high intrinsic clearance (46.03 mL min−1 kg−1) of ZNB revealed that ZNB shares similarities with medications that have a high extraction ratio. The present LC-MS/MS approach is considered the first analytical methodology for assessment of ZNB metabolic stability in HLMs matrix. In silico data from WhichP450 and DEREK modules suggest that making small structural changes (bioisosteric replacement) to the carboxamide moiety during drug design can potentially improve the metabolic safety and stability of novel compounds relative to ZNB. These methods are essential for advancing the development of new pharmaceuticals, particularly in enhancing metabolic stability.
Abstract
Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. fruits (ESF) is a natural health food that has been widely used in traditional medicine. This study aimed to establish and validate a rapid and sensitive method for determining of six phenolic acids in plasma of normal and T2DM rats by ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Separation and quantification were performed on a Waters HSS T3 column (100 × 2.1 mm, 1.8 μm) with water (A) and methanol (B). The electrospray ionization (ESI) source was operated in negative ionization mode. Multiple reaction monitoring (MRM) was used to quantitatively analyzed hyperoside m/z 463.2→301.1, caffeic acid m/z 179.1→135.1, chlorogenic acid m/z 353.2→190.9, gallic acid m/z 169.0→125.1, protocatechuic acid m/z 153.1→109.1, and isofraxidin m/z 221.1→191.0, respectively. The hypoglycemic effect of ESF was verified by determining blood glucose and lipid levels in a type 2 diabetes model. This study laid the foundation for exploring ESF clinical guidelines in the future.
Abstract
High Performance Thin Layer Chromatography has capacity to run many samples simultaneously and its reduced solvent usage. Simultaneous quantification of gallic acid, ferulic acid, rutin and berberine in Asthimajja Pachak Kwath has been developed and validated using a specific, precise, accurate, and low-cost high performance thin layer chromatography technique. Toluene: ethyl acetate: chloroform: methanol: formic acid (5:2:2:2:1, v/v/v/v/v) was used as mobile phase during separation, which took place on a stationary phase of pre-coated silica gel aluminum plate 60 F254. At 270 nm, separated components were densitometrically measured. The method was validated for linearity and range, precision, reproducibility, specificity, robustness, accuracy, limit of detection and limit of quantification as per International Council for Harmonization Q2 (R2) guideline. Gallic acid, ferulic acid, rutin and berberine regression coefficients (R 2) were found to be 0.9995, 0.9990, 0.9985 and 0.9997 accordingly. Gallic acid, ferulic acid, rutin and berberine percentage recoveries were measured to be 99.81 ± 0.833, 99.15 ± 0.776, 99.56 ± 0.582 and 99.90 ± 0.719 respectively. Having a reliable analytical method is essential for ensuring the quality, consistency, and efficacy of herbal formulations in traditional medicine. This meticulous approach is crucial for accurate quantification of the target compounds in the Asthimajja Pachak Kwath.
Abstract
Nowadays, drone imagery is a common way to quickly obtain information on the state of vegetation, as well as a method for taking orthophotos and terrain models. For terrain modelling, aerial photographs are required to have at least 60% overlap between adjacent images. Typically, the inadequate overlap is only discovered later, during post-processing. In our previous work we have presented a method we developed to determine on the spot, whether the in-flight images are suitable for producing the terrain model or whether it is necessary to re-render a part of the area, which can be done under the same conditions (weather, ionosphere, satellite geometry). Our proposed method for calculating the overlap is different from the usual procedure. Using VBA-based calculations, we computed the overlap between the images based on the position of the centre of the images, the altitude of the flight and the rotation angle of the images. The method was tested in practice, but we felt it necessary to verify our calculations. During the verification, we checked the VBA-based calculations using a Python script. The test showed that the results obtained with a previous midpoint calculation method were 92.2 percent identical to the calculations performed with Python. The Python program is accurate and fast; therefore, the use is recommended on the field.
Abstract
Similar to other regions, in East Central Europe, agriculture is the most vulnerable sector regarding the consequences of climate change through increasing variability in weather conditions, even on the short-term and local scales. Agricultural engineers make decisions; higher education has a crucial role in taking proper actions. Our survey aimed to get up-to-date information on the knowledge and attitude of graduating students completing agriculture-related studies at 6 universities located in Hungary, the Czech Republic, Poland, and Slovakia, with particular attention to weather projections, crop production, and soil protection issues. Analyses revealed adequate lexical knowledge of young engineers in each country. They are familiar with the agro-environmental actualities and future trends, issues to address at the right time, and the repertoire of tools and practices for taking efficient measures. A positive attitude toward proactive actions was proved. We report proof of a high level of preparedness resulting from the proper efficacy of agricultural higher education. The content of the curricula and the teaching methodologies meet well the receptiveness to learning in the V4 countries. Our findings confirm that frequent updating of the content of subjects as well as incorporating practical applications that promote active learning and engagement, are more critical today than ever, and it is possible to achieve a high level of preparedness for the challenges in the agricultural sector.
Abstract
This study analyzed the impact of storing Golden Delicious apples at 3 °C with a relative humidity of 85 ± 5% in two environments, namely a darkroom (D03) and a lightroom (L03), on the fruit quality. The research evaluated weight loss (Δm) and color metrics (a*, b*, L*, ΔE, C*, hue angle). The number of apples used for each storage was 12. Weight loss was calculated by measuring the changes in mass during storage. Color differences (ΔE), chroma (C*), and hue angle were determined based on the L*a*b* scale values. Apples stored at 3 °C in D03 experienced a minimal percentage of weight loss of 7.02%. The results indicated that compared to the D03 storage, the L03 storage had a more significant increase in Δm and color variation. The non-destructive method of measuring color characteristics facilitates the assessment of the storage conditions for Golden Delicious apples.
Abstract
Nutritional information on packaging is becoming increasingly important in the food industry. Currently, labels are seen not only on the back of the packaging but also on the front. As there are many versions of front-of-pack labels (FoPLs), the research aims to determine which helps consumers the most in making decisions about which food to include in a healthier lifestyle. Nutri-Score, Guideline Daily Amount (GDA) and Multiple Traffic Lights (MTL) FoPLs on cereals were compared using eye-tracking (ET) and choice-based conjoint analysis (CBCA). CBCA was used to assess consumer preferences and the labels and products were also ranked. Based on the results, GDA type FoPL proved to be the most useful based on conjoint analysis, ranking and the analysis of ET parameters. This label helped participants the most in choosing the product that best fits into a healthier lifestyle. The Nutri-Score label, which offers little information on a product's nutritional content, was not favourably received by the Hungarian sample, who preferred more detailed FoP labels.
A vízpótlás talajvízszintre gyakorolt hatásának értékelése egy délnyugat-magyarországi példán keresztül
Evaluation of the water supply’s impact on groundwater levels, with an example from South-West Hungary
Az Európát is érintő jelenlegi, napjainkban zajló éghajlatváltozás statisztikailag szignifikáns felmelegedési tendenciával jellemezhető. Az éghajlatváltozás hatása a csapadékviszonyok és az evapotranszspirációs folyamatok megváltoztatásán keresztül érinti a vízkörforgalmat, így a csapadék eloszlásának és mennyiségének várható változásai a folyamatosan emelkedő hőmérséklettel együtt a növények nagyobb vízfelhasználását eredményezhetik, ami változásokat indukálhat a talajnedvességben, a talajvízben és ennek következtében a vízmérlegben. Az emelkedő hőmérséklet hatására a jövőben a növekvő transzspirációs igény valószínűleg a növényi közösségek fokozott talajvízfelvételét eredményezi, ami a talajvízszint további csökkenését is magával vonhatja. Ha ez bekövetkezik, a talajvízfüggő erdei közösségek regenerálódása ezeken a területeken kérdésessé válik, mivel a fiatal fák gyökérzete nem fogja tudni elérni a vízforrást. Következésképpen a Kárpát-medence sík vidékein és vizes élőhelyein a nagy vízigényű erdők fennmaradása kérdésessé válhat. A fás vegetáció számára kiemelten fontos a talajvíz szerepe a vegetációs időszakban, éppen ezért a talajvízszint változását régóta, rendszeresen monitorozzák.
Konkrét megoldás lehet az árhullámok visszaduzzasztásából származó vízpótlás. A pozitív vízpótlási beavatkozásokra példa a Kaszó LIFE projekt. A projekt célja a leromlott élőhelyek rehabilitációja volt, ami a kedvező ökológiai állapot stabilizálásával teszi lehetővé a hosszú távú megőrzést. A megvalósítás eszközeként tórehabilitációt és folyó-mederbordákat alkalmaztak, biztosítva a Szentai-erdő (Nyugat-belső-somogyi kistérség) erdeinek, kis lápjainak és gyepterületeinek vízellátás javítását.
Jelen kutatás célja pedig a Kaszó LIFE projekt vízpótlási beavatkozásai után, azok felszín alatti vízszintre gyakorolt hidrológiai hatásainak elemzése volt. A meteorológiai adatok és a monitoring adatok alapján elmondható, hogy a Szentai-erdőben 30 éves szárazodási tendencia volt tapasztalható, amelynek elsődleges mutatója a talajvízszint csökkenése. Kiemelendőek a 2016–2017-es vizsgálati időszak évei, amikor az alapvetően lefolyástalan vizsgálati területen nem volt elegendő csapadék a talajvíz szintjének fenntartásához. Kutatási eredményeink azonban azt mutatták, hogy a vízpótlást célzó beavatkozások (mederbordák és tározótavak) összességében a talajvízszint emelkedését biztosítják.
A két beavatkozási típus talajvízszint emelkedésére gyakorolt hatását vizsgálva arra a következtetésre jutottunk, hogy míg a tavak építése jelentősen befolyásolja a környező kutak vízszintjét, addig a mederbordák esetében kisebb mértékű a hatás.
This study explored the effects of salicylic acid on the growth and biochemical responses of peppermint (Mentha piperita L.) under different soil salinity levels, a major challenge in agricultural productivity. The experiment was conducted using a factorial design with salicylic acid applied at concentrations of 0, 5, 10, and 50 ppm, combined with sodium chloride-induced salinity at 0, 1,000, 2,000, and 3,000 mg kg–1 soil. Results demonstrated that increasing soil salinity negatively impacted plant growth, reducing plant height, leaf number, and the dry weight of aerial parts. Salinity stress also led to reduced nutrient uptake, particularly for essential elements like calcium and potassium, while increasing sodium levels in plant tissues. However, the foliar application of salicylic acid, especially at 50 ppm, significantly improved growth parameters and mitigated the detrimental effects of salinity. Notably, at the highest salinity level (3,000 mg kg–1), salicylic acid enhanced plant height by 11.1% and leaf number by 30.9% compared to untreated plants. Salicylic acid also boosted biochemical responses, such as increasing total phenolic and flavonoid content, which are critical for stress tolerance. This study underscores the potential of salicylic acid as a stress mitigator, promoting better growth and physiological resilience in peppermint under saline conditions, offering valuable insights for improving crop performance in salinity-affected regions.
Abstract
The simplest way to remove pesticide residues from fruits and vegetables is to wash them with tap water. However, this method is not effective enough. In this study, the effectiveness of different washing methods assisted by ultrasound on pesticide removal was investigated. For this purpose firstly, apples were soaked in a cypermethrin (CYP) and spirotetramat (SPI) solution, which are frequently used as insecticides. Subsequently, the apples were washed in solutions prepared with vinegar, lemon juice, and baking soda at different concentrations (0.5%, 1% and 2%) and assisted by ultrasound (2.5–5 min). The residues in the medicated and washed samples were analysed on an LC-MS/MS instrument after extraction using the QuEChERS extraction method. The results of the analysis showed that acidic vinegar and lemon juice were more effective than baking soda. Moreover, the application of ultrasound significantly increased this effect. When a 0.5% vinegar solution was assisted by ultrasound, 62% of the cypermethrin residue was removed and 82% of the spirotetramat residue was removed. These values were 51.5% and 49.6% higher than tap water, respectively. In conclusion, acidic solutions such as vinegar, which we can easily prepare at home, are highly effective in removing pesticide residues when assisted by ultrasound.
Abstract
The relevance of the subject under study is conditioned by numerous technological problems of providing livestock enterprises of the Republic of Kazakhstan with quality equipment for animal feeding and the associated need to develop and implement dosers for the preparation of compound feed mixture. This study introduces an innovative approach through the development and analysis of a novel dosing auger with an active return channel, which distinguishes itself from existing models by enhancing the precision and efficiency of feed preparation processes. The purpose of this study was to investigate the key parameters of the dosing auger with an active return channel for its further use in agricultural enterprises for preparation of compound feed. The findings of this study emphasise the significance of compliance of current trends in the improvement of prepared feed with the established zootechnical requirements from the standpoint of optimising the technological equipment used in this process. The key aspects of feed dosing sequence when using volumetric and mass dosing methods were considered. The main advantages of auger-in-auger dosers that distinguish them from all other types of dosers were described.
Abstract
Dillenia indica is one of the important medicinal plants and is extremely popular in many systems of medicine including ayurvedic, homeopathic, and siddha. Traditionally, different parts of this plant have been used to treat cancer, wound healing, diabetes, diarrhea, bone fractures, abdominal pains, cuts and burns. In the present study, a simple, precise, accurate and validated high performance thin layer chromatographic (HPTLC) method was developed for simultaneous estimation of three pharmaceutically active compounds i.e., betulinic acid (BE), β-sitosterol (BT) and lupeol (LP) in fruits, leaves, root bark and stem bark of D. indica. Standards and plant samples were applied on TLC aluminum plate precoated with 0.2 mm layer of silica gel 60F254. The plate was run in a twin glass chamber comprising toluene:methanol:chloroform (8:1:1, v/v/v) as a mobile phase which resulted in better separation of compounds. The plates were immersed in anisaldehyde-sulfuric reagent and then heated at 105 °C for 5 min in CAMAG TLC plate heater for appearance of bands. Densitometric scanning was performed at λmax = 525 nm using tungsten light source in CAMAG TLC Scanner4 armed with WinCATS software. R F values of BE, BT and LP standards and those of plant samples were found to be 0.38 ± 0.01, 0.54 ± 0.01 and 0.65 ± 0.02 respectively. The method was further validated by following the International Conference of Harmonization (ICH) guidelines. For BE, BT and LP, the linear regression data for the calibration plots revealed a satisfactory linear association with correlation coefficients (r 2) = 0.9736, 0.9989 and 0.9957, respectively. Linear ranges for BE, BT and LP were 2,000–6,000 ng/band, 200–1,000 ng/band, and 200–600 ng/band respectively. Accuracy of the method was assessed by recovery study conducted at three different levels with the average recovery of 99.19, 99.69 and 100.95% for BE, BT and LP, respectively. The results exhibited the highest content of BE (0.148 ± 0.01%), BT (0.031 ± 0.01%) and LP (0.047 ± 0.01%) in stem bark. The developed method will be useful for routine and quality control analysis of fruits, leaves, root bark and stem bark of D. indica species.
Abstract
Artificial sweeteners are low-calorie substances used as food additives with aim to impart a sweet taste to beverages without adding significant calories. Due to the regulatory compliance regarding the type and the amount of artificial sweetener, and due to the large consumption of beverages and the effects of artificial sweeteners on human health, their identification and quantification is of a great importance. In this research simultaneous determination of acesulfame K (ACE-K), sodium saccharin (Na-SAC) and aspartame (ASP) as the most commonly used sweeteners in beverages was performed with a reversed – phase high performance liquid chromatography (RP – HPLC) with diode array detection (DAD). The best separation of the analytes was achieved on a Poroshell 120 EC-C18 (3.0 × 50 mm, 2.7 µm) column and isocratic elution with a mobile phase consisted of acetonitrile and diluted phosphoric acid (pH = 3.8) with 7/93 volume ratio (V/V), and flow rate of 1 mL min−1. The chromatographic process was followed at 195, 220 and 230 nm, under constant column temperature (25 °C). Under these chromatographic conditions, the total time of analysis was less than 5 min. The developed method was validated for linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The LOD under established chromatographic conditions was 0.03, 0.07 and 0.17 mg L−1 for Na-SAC, ACE-K and ASP, respectively. The amount of artificial sweeteners in analyzed samples ranged from 30.32 to 148.37 mg L−1 for ACE-K, from 16.10 to 93.05 for Na-SAC, and from 6.06 to 512.72 for ASP. The validated method was successfully applied for determination of analytes in different commercially available beverages.
Abstract
People are consuming increasing amounts of poultry eggs and their products, and their safety is always a public concern. However, the complex composition of poultry eggs and their products, particularly the proteins and lipids, can easily cause matrix effects, requiring the use of sorbents to remove these components to avoid affecting the detection results. Zeolitic imidazolate framework-8 (ZIF-8) is a MOF material with high specific surface area, high porosity, and high stability, making it widely used as a sorbent in pesticide residue detection. In this study, we evaluated the performance of ZIF-8 compared to classic solid phase extraction (SPE) and Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) in the pretreatment step. The results showed that ZIF-8 could better reduce the matrix effect in poultry eggs and their products. After optimizing the extraction solvents, chromatographic and mass spectrometric conditions, and pretreatment processes, we established a method using ZIF-8 as a sorbent combined with high performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) for the detection of 80 pesticide residues in seven different types of poultry eggs and their products, yielding satisfactory results. All the target analytes showed good linearity, both with values of r 2 > 0.996. The average recovery and coefficients of variation (CVs), expressed as relative standard deviations, ranges from 72.5% to 113.2% (chicken egg) (CV: 0.1%–12.9%), 72.2%–114.2% (salted duck egg) (CV: 0.1%–9.8%), 70.3%–105.6% (goose egg) (CV: 0.1%–12.0%), 70.9–120.4% (marinated egg) (RSD: 0.1%–14.8%), 70.7%–108.5% (duck egg) (CV: 0.1%–12.3%), 71.1%–105.0% (quail egg) (CV: 0.2%–5.6%), 70.7%–111.5% (century egg) (CV: 0.1%–13.4%). The values of limit of detection (LOD) and limit of quantification (LOQ) were, respectively, ranging from 0.15 to 0.85 μg kg−1 and 0.34–2.6 μg kg−1. When this method was applied to the detection of real samples, one chicken egg sample was found to contain 0.013 mg kg−1 of fipronil, and one marinated egg sample was found to contain 0.0087 mg kg−1 of thiamethoxam, indicating the necessity of stringent safety monitoring for poultry eggs and their products.
Abstract
Formaldehyde plays a significant role in the global economy due to its unique chemical properties and widespread use in both the medical field and various industrial sectors. However, formaldehyde (HCHO) is classified as a persistent organic pollutant and is known to be harmful. Exposure to formaldehyde, both direct and prolonged, can cause severe health issues and potentially lead to death. It is recognized as a human carcinogen by numerous organizations and can negatively impact the endocrine system, as well as having mutagenic or teratogenic effects. Formaldehyde has been detected in various matrices at levels exceeding those permitted by international health regulatory bodies. Chromatography, particularly high-performance liquid chromatography (HPLC) coupled with detection methods, is an analytical technique frequently used to determine volatile organic molecules, including formaldehyde. This investigation aimed to develop and validate an assay method to identify and quantify formaldehyde in cosmetic products using HPLC-PDA. The chosen isocratic system consisted of a ZORBAX RX-C8 column (250 mm × 4.6 mm; 5 μm) and a mobile phase mixture of acetonitrile and water in a 55:45 (v/v) ratio, with a flow rate of 1.5 mL min−1. Formaldehyde was detected at 353 nm after derivatization with a 0.1N 2,4-dinitrophenylhydrazine solution, with a retention time of approximately 5.0 min and a total run time of 7.0 min for formaldehyde. The method was validated according to ICH Q2 (R1) guidelines. The validation parameters demonstrated high selectivity, precision (RSD <2%), accuracy (mean recovery of 101.3%), linearity (r > 0.995 in the 1,000–2,400 ppm range), and a limit of quantification (LOQ) of 0.1 ppm. The validated analytical method was applied to 35 cosmetic products. None of these products were labeled as containing formaldehyde, although 6 imported products were labeled as containing formaldehyde-releasing preservatives. The results indicated that 88.6% of the samples tested positive for formaldehyde, with free formaldehyde levels ranging from 20 to 981 ppm. All samples contained formaldehyde levels below the 2000 ppm threshold.
Abstract
Currently, there are no reported green “high-performance thin-layer chromatography (HPTLC)” methods for domperidone (DOM) and cinnarizine (CNZ) simultaneous detection. The objective of the present study was to design and verify a reverse-phase HPTLC method for the concurrent analysis of CNZ and DOM in commercial tablets that is fast, sensitive, and greener. As a green mobile phase, acetone and water in an 80:20 (v/v) binary ratio were used to simultaneously determine CNZ and DOM. The stationary phase was reverse-phase silica gel 60F254S plates. Concurrent measurements of CNZ and DOM were performed at 230 nm. Four different tools were used to assess the greenness of the current method: AGREE, AES, ChlorTox, and NEMI. For both medications, the current approach was linear in the 25–1,000 ng/band range. The accuracy, precision, robustness, sensitivity, and environmental friendliness of the suggested technique for the CNZ and DOM simultaneous detection were verified. The new method's profile was noticeably greener, as seen by the results of every greenness tool, including NEMI, AES (89), ChlorTox (1.08 g), and AGREE (0.83). Utilizing the current approach, the amount of CNZ and DOM in pharmaceutical tablets was found to be 99.53 and 98.87%, respectively. These findings validate the suitability of the existing method for measuring CNZ and DOM simultaneously in commercial tablets. The results of the proposed study indicated that measuring CNZ and DOM in commercial products could be done consistently with the current methodology.
Abstract
A fast, accurate, sturdy, and sensitive UPLC-MS/MS method was developed to measure the levels of ADB-BUTINACA in rat plasma for a pharmacokinetic study. The ADB-BUTINACA and midazolam (internal standard) were separated on a UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using a gradient elution of acetonitrile and water (0.1% formic acid) as the mobile phase. ADB-BUTINACA and midazolam were detected in multiple reaction monitoring (MRM) mode for quantitative analysis, the mass detection was performed on a positive electrospray ionization (ESI) source. The calibration curve displayed excellent linearity from 1 to 1,000 ng mL−1, with a lower limit of quantification of 1.0 ng mL−1 and a limit of detection of 0.3 ng mL−1. The precision for both inter-day and intra-day assays was below 14%, while accuracy ranged from 92% to 111%. The method also showed an average recovery between 87% and 90%, with a matrix effect ranging from 104% to 111%. The data was acceptable according to the guidelines of the US Food and Drug Administration (FDA). This newly validated quantitative method successfully supported the pharmacokinetic study of ADB-BUTINACA.
Abstract
In the confectionery industry large quantities of palm fat in the fillings of chocolate products are used. Based on today's nutritional science results, it is desirable to replace palm oil with healthier fats. Oleogels can provide a kind of solution for this replacement. In our work the rheological, textural and thermal properties of oleogels containing high oleic sunflower oil, beeswax and monoglycerides were determined. In the samples we examined, the gelator concentrations were: 20% beeswax, 15% beeswax and 5% monoglyceride, 10% beeswax and 10% monoglyceride, 5% beeswax and 15% monoglyceride, and 20% monoglyceride. Based on our results, the oleogel containing 15% beeswax and 5% monoglyceride seems an eutectic crystal of beeswaxes and monoglyceride. It has relative high hardness, high storage modulus and high viscosity therefore it can replace the Chocofill filling fat, which contains mainly palm fat, used in large quantities in sweets.
Abstract
The use of edible coatings (ECs) containing essential oils (EOs), such as that derived from the Thymus vulgaris plant (EO-Tv), offers a natural option for preserving and increasing the shelf life of fruit and vegetable products. However, considering their physicochemical properties, the incorporation of EOs into nanocapsules (NCs) represents an alternative to reduce their volatility and oxidation. In this way, quantitative determination of the EOs incorporated into NCs is necessary for simultaneous monitoring of their main components during the nanoencapsulation process, as well as for the future precise and accurate dosage of EO components in fruit and vegetable products. In this study, ECs were formed from NCs loaded with EO-Tv and sodium alginate (AL). The EO-Tv was characterized through GC-MS and GC-FID analysis, and it was found that the major component of EO-Tv was thymol, with an abundance of 30.91%. Subsequently, an analytical method based on HS-SPME-GC-FID was developed and validated for quantification of the EO-Tv encapsulated in NCs and incorporated into the EC. The method was found to be precise and accurate for quantification of the main components of EO-Tv in the formed EC. Once the analytical method was validated, it was established that the encapsulation efficiency was greater than 50% in the case of NC-EO-Tv purified via evaporation at reduced pressure. On the other hand, 35.78 μg cm−2 of thymol was quantified in the EC formed from the NCs and AL. The present work presents an analytical tool for simultaneous quantification of the main components of EO-Tv in NCs, as well as in the ECs formed with NCs, promoting its potential application in fruit and vegetable products.
Abstract
The spray is the primary method to apply pesticides to the crops. To provide enough coverage and deposition on target surfaces, the drop size produced during spray application must be precisely calibrated; nevertheless, it must not be too tiny to cause the undesirable phenomena known as “spray drift”. Spray drift is the movement of droplets in the atmosphere during or after spraying. The negative effect of spray drift can harm human health, livestock, and adjacent crops or can cause environmental pollution. To address this problem, a lot of work has been done. Previous studies on spray drift reduction approaches including factors promoting drift, drift measuring technologies, drift prediction models, and drift reduction technologies, were reviewed in this paper. Based on the literature review, future research and developments are projected. This review may provide guidance and reference to researchers for further development and improvement in drift reduction technologies.
Abstract
Sumiprempt containing Pyriproxyfen and fenpropathrin insecticides is used for pest control in okra crop. Pyriproxyfen can disrupt endocrine function, while fenpropathrin disrupts voltage-gated sodium channels in neurons. Based on their health risk to consumers and impact on environmental deposition, an experiment under field was planned to evaluate deposition, decontamination and related dietary risks. A methodology was developed and validated to identify and quantify the pyriproxyfen + fenpropathrin residues, extracted via QuEChERS method using GC-MS/MS. The foliar application of ready-mix formulation (Pyriproxyfen 5% + Fenpropathrin 15% EC) @ 750 gm mL−1 ha−1 and 1,500 gm mL−1 ha−1 leads average initial deposition pyriproxyfen 5% (0.359, 0.584 ppm) and fenpropathrin (0.643, 1.005 ppm) at respective doses. Residues reached below limit of quantification (0.01 ppm) on 15th and 20th day for pyriproxyfen and 10th and 15th day for fenpropathanin at the recommended and double the recommended doses, respectively. Dissipation followed the first-order kinetics with half-life value ranged in between 1.79–1.84 (pyriproxyfen) and 2.27–2.31 days (fenpropathrin) at the respective doses. The pre-harvest interval of 12 days was recommended for safe consumption of okra fruit. Even though all the decontamination treatments were successful in lowering the residues of both chemicals to substantial levels, washing followed by boiling was found to be the most effective treatment for reducing the residues. The risk quotient values were less than 0.01, implying that pyriproxyfen and fenpropathrin offer no dietary risk to consumers.
