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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 prevalence of diabetes is increasing day by day as per a report by the year 2045, 1 out of every 8th individuals may suffer from diabetes. This research article focuses on developing and validating Metformin and Dapagliflozin in combination by using high-pressure liquid Chromatography (RP-HPLC). The validation of the method was followed as per the guidelines provided by the International Conference on Harmonization (ICH) and United States Pharmacopeia (USP). Separation of both drugs takes place in less than 4 min. This separation takes place using Phosphate buffer (pH 6.8) and acetonitrile in a 45:55 (v/v) ratio at a 1.0 mL min−1 flow rate. Furthermore, studies on both drugs were conducted by using the bulk and pharmaceutical dosage forms (Tablets). The developed method was accurate as drug recoveries in both cases of Metformin, and Dapagliflozin ranged between (100.8, 99.6, 98.8%) to (100.8, 99.3, and 101.5%) respectively having a concentration range of solutions between 70, 100 and 130 μg mL−1 dilution. The recommended method for simultaneous quantification of Metformin and Dapagliflozin was established and validated and no excipient interactions were found.
Abstract
This study investigates sustainable methods for producing protein from soybean expeller via pH-shifting processes, aiming to reduce water usage in alkaline extraction by adjusting solid-to-liquid ratios per cycle and employing isoelectric precipitants like lactic acid and lactic acid bacteria (Lactiplantibacillus plantarum and Lactococcus Lactis) to enhance functional and antioxidant properties over a wide pH range. Results indicate that the most efficient approach involves three 1:10 (w/v) extraction cycles with lactic acid bacteria as precipitants, demonstrating high productivity and low specific water consumption. Protein content and recovery yield showed no significant differences compared to alternatives with higher water consumption or less eco-friendly precipitants. Despite lower solubility, protein products precipitated with lactic acid bacteria formed stable emulsions, exhibiting superior free radical scavenging activity.
Abstract
Microencapsulation of flaxseed oil (FO) has received lots of attention in the food and biopharmaceutical industries. To produce FO microcapsules, aqueous emulsions of FO with polymeric carbohydrates (maltodextrin (MD) with dextrose equivalent (DE) 19, gum Arabic (GA) and modified starch (MS)) were prepared by a rotor stator homogenization and subsequently, dehydration of emulsions were performed by spray drying (SD). The objective of this research was to study the effects of different combinations of polymeric carbohydrates with FO in emulsion to obtain maximum encapsulation efficiency (EE). A 3 factorials–3 levels Box–Behnken design was used for the optimization purpose. The maximum EE was achieved using 0.79 MD-GA ratio, 20.23% MS and 24.62% FO in emulsion. Microcapsules obtained by optimum condition had EE 77.68%, particle size (D 32) 120.0 ± 0.43 μm, moisture content1.6 ± 0.13%, wettability 192 ± 5.5 s, solubility 75.49 ± 1.3%, bulk density 0.31 ± 0.025 g mL−1, tapped density 0.36 ± 0.01 g mL−1, Carr's Index 13.88 ± 0.01% and Hausner Ratio 1.16 ± 0.01.
Abstract
During the testing of laboratory Voriconazole API batches, one unidentified impurity (IMP-5.312) was detected employing the Pharmeuropa HPLC technique at a level in excess of 0.10%. This IMP-5.312 was synthesized and then characterized as 6-(3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl) butan-2-yl)-5-fluoropyrimidin-4-ol by the corresponding spectral information (MS, 1H-NMR, 13C-NMR, and IR). The IMP-5.312 impurity was effectively quantified using an enhanced HPLC based-technique that was developed as well as validated. The approach made use of a Novapak C18 column with an inner diameter of 3.9 mm and a length of 150 mm (4.0 µm) for chromatographic separation. The analysis of IMP-5.312 was made at 45 °C, with a flow rate (isocratic) of 1.0 mL min−1 and a 256 nm detection wavelength. Acetonitrile, methanol, and 0.1% aqueous trifluoro acetate buffer (pH 4.0) were mixed at a ratio of 15:30:55 (v/v/v) to create the mobile phase for a 20 μL sample injection. The linearity range of 0.25281–1.51690 μg mL−1 had a correlation coefficient more than 0.99942, and the accuracy ranged from 89.3 to 100.3%. It was noted that the established HPLC based-technique was sensitive, specific, and precise. The technique was executed on the current batches of VRC API for IMP-5.312 analysis, and the outcomes were good. For quality control purposes during the manufacturing procedure of VRC, the identification as well as analysis of IMP-5.312 should be helpful. The in silico approach was applied to predict the IMP-5.312 toxicity. The reports indicated that IMP-5.312 in non-mutagenic and categorized as ICH M7 class-5 impurity.
Abstract
In this investigation, a rapid and reliable ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) technique was developed for quantification of veliparib in rat plasma and used the method to study the pharmacokinetics and bioavailability of veliparib in rats after oral (6 mg kg−1) and intravenous (2 mg kg−1) administration. Plasma samples were protein precipitated with acetonitrile using midazolam as internal standard. A UPLC HSS T3 chromatographic column was utilized for separation, with a mobile phase consisting of methanol-water-formic acid in gradient elution procedure. Quantitative analysis was performed using multiple reaction monitoring in electrospray positive-ion mode. Veliparib exhibited excellent linearity within the 1–1,000 ng mL−1 range (r > 0.99). The intra- and inter-day precision of veliparib were both within 15%, and the accuracy ranged from 93.7 to 107.7%. The average recovery was above 86%, and the matrix effect was 89.0–95.8%. The AUC(0-t) values for oral and intravenous administration were 1014.7 ± 42.9 and 647.2 ± 85.2 h ng mL−1, respectively, resulting in a bioavailability of 52.3%. The UPLC-MS/MS method established in this study featured a low sample injection volume, a low quantification limit, a short chromatographic runtime, high sensitivity, and selectivity. The developed method can be used for the pharmacokinetic analysis of veliparib in both preclinical and clinical studies.
This study assesses the elemental composition of Egyptian glauconite sediments, focusing on potentially toxic elements (PTEs) and macronutrients. The primary aim is to evaluate the feasibility of utilizing these sediments as a natural source of potassium for agricultural purposes, besides conventional chemical fertilizers like potassium sulfate. To quantify elemental content, chemical analysis was employed across five distinct grain size fractions after grinding glauconite rock. The assessment included potassium, calcium, sodium, and PTE concentrations, utilizing potassium chloride (KCl) and ammonium acetate lactate (AL Solution) as single extractants, and the BCR extraction protocol, in addition to measuring the pseudo-total content of these elements. Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) facilitated a comparative analysis of elemental concentrations. Results indicate PTE concentrations within European Union regulations, with an absence of cadmium. Glauconite samples contain approximately 3–3.3% potassium by weight, alongside significant amounts of essential macronutrients (calcium, magnesium) and micronutrients (copper, nickel, zinc) crucial for agriculture. BCR sequential extraction protocol results closely align with or slightly surpass pseudo-total content results. Notably, the AL Solution demonstrates high efficiency compared to KCl or acetic acid in the first step of the BCR method. BCR sequential protocol provides valuable insights into various elemental forms and potential mobility. Overall, this study reveals that glauconite has the potential to serve as a promising alternative potassium fertilizer without causing adverse environmental impacts.
Abstract
Monitoring medications in biological fluids is an essential aspect of patient care, particularly in cases of altered mental status where accurate diagnosis, effective treatment, and even forensic examinations are crucial. In this study, a new approach combining hydrophobic-deep-eutectic and solvent-bar-microextraction (HDE-SBME) followed by a high-performance liquid chromatography-diode array detector (HPLC-DAD) was developed for the simultaneous determination of desipramine, clomipramine, as antidepressant and carbamazepine as antiepileptic agents in untreated human urine and plasma samples. The HDE solvents, synthesized using various ratios of menthol and fatty acids, were utilized in the SBME setups. Computational methods were employed to predict the structure and modes of interaction between HDE and the chosen analytes. Central composite design methodology (CCD) was used for multivariate optimization of the effects of different parameters influencing the extraction efficiency of the proposed method. Under optimized experimental conditions, the calibration graph of the spiked selected drugs in urine and plasma samples demonstrated excellent linearity (R 2 ≥ 0.994), with limits of detection/quantification below 0.60/2.02 μg L−1. The extraction recoveries achieved were 88–97%, and the repeatability/reproducibility (RSD%, n = 5) was less than 6.12/7.57. The proposed method was successfully applied to determine selected drugs in patients' urine and plasma samples. The proposed method detects three drugs in patients' urine and plasma samples without using toxic volatile organic solvents. The proposed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity compared with other published methods. Thus, it can be considered a promising method for monitoring the therapeutic levels of specific antidepressant and antiepileptic drugs in urine and plasma samples.
Abstract
The primary objective of the present inquiry is to formulate a sustainable method employing Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) for determination of Amlodipine (AM) and Irbesartan (IRB) simultaneously, compounds commonly prescribed for hypertension treatment. Existing literature underscores the absence of a comprehensive method in this regard. This research endeavors to align with the tenets of green chemistry by seamlessly integrating Analytical Quality by Design (AQbD) with RP-HPLC, replacing environmentally hazardous chemical modifiers with eco-friendly solvents. Identifying the critical variables as the 70% ethanol level and flow rate, a central composite design is applied for optimization. The separation is achieved utilizing a Phenomenex Luna column (C 18 , 250 mm × 4.6 mm i.d, 5 μm) with a mobile phase comprising ethanol and 0.1 % o-phosphoric acid in a 70:30 v/v ratio, flowing at 0.8 mL min−1, and detection wavelength of 242 nm. Green assessment methodologies are implemented to gauge the adherence of the proposed RP-HPLC method to eco-friendly principles while ensuring efficiency in chromatographic performance. The current developed method is rapid with retention time of 2.3 and 3.3 min for AM and IRB respectively and having a wide linear range from 55 to 130 μg mL−1, which makes the suitable for the accurate quantification of AM and IRB simultaneously in bulk and tablet dosage form, there by minimize environmental impact by providing a conscientious choice for the routine analysis which is achieved through the amalgamation of AQbD with a sustainable approach.
Abstract
SZJ-1207 is a natural product extracted from Stephanotis mucronata (Blanco) Merr which has significant antidepressant effects in various depression mouse models, without obvious acute toxicity or sedative-hypnotic side effects. The aim of this study was to preliminarily clarify the pharmacokinetic characteristics of SZJ-1207 in rats after a single intragastric and intravenous administration. In this study, sensitive and reliable UPLC-MS/MS quantification methods were established and then successfully applied to the pharmacokinetic study of SZJ-1207 in rats. The linear range of SZJ-1207 were 0.5–400 ng mL−1 in plasma, feaces, bile and 20–4,000 ng mL−1 in urine, respectively (r > 0.99). All methods met the requirements of ICH M10. The results of pharmaconetic study showed that Cmax, AUC(0-t) and AUC(0-∞) had linear relationships with the administered doses in the range of 0.5–4.5 mg kg−1. There was a significant gender difference in the AUC (0-t) of 0.5 and 1.5 mg kg−1 and Cmax of 1.5 mg kg−1 after ig (P < 0.05). The excretion rates of SZJ-1207 were 8.46 ± 4.82% in feces, 1.89 ± 1.08% in urine, and 0.179 ± 0.118% in bile. The oral absolute bioavailability of SZJ-1207 was calculated as 64.64%.
Abstract
Objective
The levels of fraxetin, fraxin, and dimethylfraxetin in rat plasma to be measured using an ultra-performance liquid chromatography tandem mass-spectrometry (UPLC–MS/MS) technique and applied to their pharmacokinetics and bioavailability.
Methods
The protein precipitation technique was applied to the plasma preparation using acetonitrile and methanol (9:1, v/v). At a flow rate of 0.4 mL min−1, the elution time was 6 min. The mobile phase consisted of acetonitrile-water with 0.1% formic acid, and the chromatographic column was UPLC HSS T3 (50 mm × 2.1 mm, 1.8 μm). Quantitative analysis was conducted using multiple reaction monitoring (MRM) mode and detection was performed using electrospray ionization (ESI) positive ion mode. In each group, six rats were treated with fraxetin, fraxin, and dimethylfraxetin either orally (5 mg kg−1) or intravenously (1 mg kg−1).
Results
The calibration curves showed good linearity in the range of 2–4,000 ng mL−1, where r was greater than 0.99. The bioavailability of dimethylfraxetin, fraxin, and fraxetin was determinated to be 19.7, 1.4, and 6.0%.
Conclusion
The established UPLC-MS/MS method for determining the levels of these three compounds in rat plasma was successfully applied to the pharmacokinetics of dimethylfraxetin, fraxin, and fraxetin, and the bioavailability was calculated.
Abstract
The article evaluates how well the goals of the European Green Deal are justified, especially considering the risks to energy and food security arising from the conflict between Russia and Ukraine. We agree with the objectives of the European Green Agreement as a whole, but whether some of the objectives which feature in the EASAC study can be achieved by 2030 is questionable, and the description of the tools necessary to achieve the objectives is incomplete. Among other things, there is hardly any mention of the role played by precision farming with digitalization, which is a revolutionary change from an ecological and economic point of view, in reducing the use of synthetic inputs, in regenerating the original state of the soil, in reducing GHG emissions, thus in increasing biodiversity, and at the same time in intensifying production, and finally in expanding the application of biotechnology. We examine these areas in our analysis. Some of the objectives of the EASAC study to be achieved by 2030 are subject to debate, and the description of the information and communication conditions necessary to achieve the objectives is incomplete. The IoT (Internet of Things) responds to global and local challenges: it integrates the precision technologies, WSNs (Wireless Sensor Networks), artificial intelligence, mobile field (Smart Small Robots) and remote data loggers (UAVs: Unmanned Air Vehicles and satellites), Big Data, and cloud computing. Consequently, decision support is increasingly developing into unmanned decision making. IoT (Internet of Things) is the basis of “Farm to Fork” and “Lab to Field” monitoring approaches.
This article evaluates the implementation of European Green Agreement objectives in light of energy and food security risks arising from the Russia-Ukraine conflict. While overall support for the agreement exists, the feasibility of certain EASAC study objectives by 2030 is called into question due to insufficient tools specifications. Notably absent is the emphasis on precision farming with digitalization, which is a transformative ecological and economic practice. Our analyses look into its function in reducing synthetic inputs, soil regeneration, GHG emission reduction, biodiversity enhancement, production intensification, and biotechnology development. Debates surround EASAC study objectives for 2030, despite limited information and communication restrictions. The Internet of Things (IoT) arises as a solution, combining precision technology, WSNs (wireless sensor networks), AI (artificial intelligence), smart small robots, UAVs (unmanned aerial vehicles), satellites, big data, and cloud computing. As a result, decision support turns toward unmanned decision-making, with IoT laying the groundwork for “Farm to Fork” and “Lab to Field” monitoring systems.
The use of organic fertilization is declining in Hungary due to the sharp fall of livestock stand since the middle of the 1980s. Most farmers are forced to use solely chemical crop enhancers. A bifactorial small plot experiment was carried out between 10 May 2023 and 19 October 2023 in Keszthely, in order to examine the effects of farmyard manure (M), green manure (GM) and stem residues (SR) on the nutrient uptake and nitrogen utilization efficiencies of maize at equidistantly increasing (0–70–140–210–280 kg N ha–1) nitrogen doses. The relationship between some vegetative traits (dry biomass weight, Leaf Area Index (LAI)) and yield, furthermore leaf relative water content (RWC) was also examined. According to the results, organic fertilizer substitution significantly increased the N content both in whole plant and grain samples of NPK+M and NPK+GM+SR treatments, compared to the chemically fertilized control (NPK). In case of P and K only slight differences were observed. Whole plant K contents of NPK+M were significantly higher than in the other treatments (P = 0.045; P = 0,005), furthermore P contents in grain samples were significantly higher in NPK+M (P = 0.004) and NPK+GM+SR (P = 0.05) than in control. Harvest index (HI [%]) of NPK+M and NPK+GM+SR were 1.06 and 1.05 times higher than in NPK. Depending on the treatment, P0023 maize hybrid absorbed 58.7–74.64% of total N uptake in the grain (HIN%), and the utilization of 1 kg N fertilizer for the extra yield above the yield of the individual control was 0.39–1.38 kg (AREN). Significant positive correlations were observed between dry biomass weight and yield (NPK: r = 0.937, P = 0.019; NPK+M: r = 0.971, P = 0.006; NPK+GM+SR: r = 0.88, P = 0.049), furthermore LAI and yield (NPK: r = 0.9, P = 0.037; NPK+M: r = 0.983, P = 0.003; NPK+GM+SR: r = 0.784, P = 0.117). Highest RWC values – which may be related to better soil aggregate stability – were measured in NPK+GM+SR treatment, therefore there may be a great potential in this treatment among drought conditions. The effect of organic amendments is particularly noticeable with smaller nitrogen doses so they should be used to reduce inorganic fertilizer application and the resulting environmental risks.
Abstract
A simple, fast and selective analytical method has been developed for the simultaneous determination of allantoin and D-panthenol in cosmetic products containing Aloe vera extracts. The proposed method depends on reversed-phase liquid chromatography with isocratic flow profile of the mobile phase composed of acetonitrile–10 mM phosphoric acid (pH 2.5) (85:15, v/v), with a C18 column at 30 °C. The analytes were detected with UV–vis. detector at 210 nm. The injection volume was 20 μL. The linearity ranges were found to be 0.2–20 and 0.1–10 μg mL−1 for allantoin and D-panthenol, respectively. LOD values were found to be 0.07 μg mL−1 and 0.03 μg mL−1, LOQ values were found to be 0.2 and 0.1 μg mL−1 for allantoin and D-panthenol, respectively. No interference was observed from concomitants. The developed method was applied to the analysis of 10 different type cosmetic products. It is foreseen that the method will be able to be used in order to carry out routine analysis, quality control and standardization in cosmetic products containing allantoin and D-panthenol.
Abstract
A simple, rapid, and green high-performance liquid chromatography-mass spectrometry (HPLC-MS) method was developed for determination of tauroursodeoxycholic acid (TUDCA), taurocholic acid (TCA), and taurochenodeoxycholic acid (TCDCA) in bio-transformed Jindanfen (BTJDF), which is obtained from chicken bile through a bioconversion process. The sample was prepared using water. The HPLC separation was operated on a poroshell 120 EC-C18 column with a 2.0 min gradient elution procedure. Detection was performed on a single quadrupole mass spectrometer in negative mode with selected ion monitoring mode (SIM). This developed HPLC-MS method presented good linearity (r > 0.997) and sensitivity (limit of quantification, 30.0–80.0 pg) for three analytes. The relative standard deviations (RSDs) for precision, repeatability, and stability were all below 3.00%. The matrix effects and average recoveries of three analytes were 91.2–97.9% (RSDs < 1.50%) and 95.4–103% (RSDs < 3.00%), respectively. The average contents of TUDCA, TCA, and TCDCA in ten batches of samples were 33.8, 13.2, and 20.5%, respectively. Finally, the greenness of the developed method was validated by Analytical Eco-Scale and Complex-GAPI. The developed method was proved to be an eco-friendly, effective, and reliable approach for assaying the three cholic acids in BTJDF, which is help to improve the quality evaluation level of the BTJDF industry.
Abstract
The current technologies for substandard and counterfeit drug detection are either too expensive for low-resource settings or only provide qualitative or semi-quantitative results. GPHF minilab™ is one of them based on thin layer chromatography(TLC) principles with a semi-quantitative capability by visual observation of the spot area and intensity for medicine quality analysis. Thus, its use as a quality control tool for pharmaceutical products has limitations as spot area and intensity visual observation by the naked eye highly varies from analyst to analyst. As such, in this study, the semi-quantitative technique has been transferred to a quantitative approach by capturing the developed TLC plate image using an Android-based mobile phone inside a simple carton box. Then, the spot area was quantified using justTLC software. The quantitative results were compared with the-high performance liquid chromatography (HPLC) method as the golden standard. Accordingly, linearity was observed in the assayed range (80–120% label claim), and the correlation coefficients found were (R 2 = 0.958, 0.997, 0.941, and 0.956 for Albendazole, Mebendazole, Artemether, and Lumefantrine, respectively.). The values are satisfactory. The %RSDs found were less than 2% for all drugs [intraday (n = 6) (RSD = 1.17, 1.61, 1.87, and 1.64), and interday (n = 18) (RSD = 1.16, 0.72, 1.12, and 1.18) for Artemether, Lumefantrine, Mebendazole, and Albendazole, respectively]. Moreover, comparisons of results obtained from the sophisticated CAMAG UV cabinet (R 2 =0.991, 0.971, 0.946, and 0.967) and the developed simple carton box (R 2 = 0.958, 0.997, 0.941, and 0.956) for Albendazole, Mebendazole, Artemether, and Lumefantrine, respectively. The values are comparable and reveal the accuracy of the method. Robustness testings' that were performed under different altered conditions revealed the robustness of the method (RSD less than 2% for all factors). Additionally the deviations from the golden HPLC results were on average −8.62% for albendazole, −3.79% for artemether, and −4.52% for lumefantrine samples. The developed method shows a satisfactory performance capability to utilize the GPHF minilab™ as a quantitative technique for medicine quality control purposes. It will be a very useful tool in a resource-limited setting. The target method profile, which encompasses a simple, low-cost, linear, precise, robust, accurate, and quantitative GPHF minilab™ system, was obtained for Albendazole, Mebendazole, and Arthemeter lumefantine combinations (Co-artem). The proposed method was successfully applied to analyze the content of the marketed medicines in the above mentioned tablets and offered acceptable deviations from the golden HPLC method. Automation of quantitative GPHF minilab™ was highly recommended to enhance the appropriateness and use of this system.
Abstract
Due to the frequent use of paracetamol formulations, it is useful to develop an analytical technique for the determination of intact paracetamol in presence of other drugs and excipients or the degradation products. In this study, a simple, isocratic, fast, specific, accurate and precise stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated for simultaneous quantitative determination of paracetamol (PCM) and potassium sorbate (PS) in oral liquid formulations. The chromatographic separation was achieved on Zorbax SB C18 column (150 × 4.6 mm, 5 µm) with Zorbax SB C18 precolumn (12.5 × 4.6 mm, 5 µm) using distilled water pH 2 with ortho-phosphoric acid and acetonitrile (70:30, v/v) as a mobile phase, and UV detection at 235 nm. The temperature of the column was kept constant at 25 °C. The method was validated according to International Conference on harmonization (ICH) guidelines. The method demonstrated excellent linearity, with a correlation coefficient of 0.9996 and 0.9998 for PCM and PS, respectively, over the concentration ranges of 10–600 μg mL−1 (PCM) and 6–500 μg mL−1 (PS). The retention time was found to be 1.98 and 4.86 min for PCM and PS, respectively. Oral liquid formulation samples were subjected to various stress conditions (acidic and alkaline hydrolysis, as well as oxidative, heat and photolytic degradation) for the purpose of forced degradation study. The major degradation of paracetamol was achieved in acidic and basic stress conditions, while thermal and photolytic degradation generally had the least influence. On the other hand, potassium sorbate was highly susceptible to photolytic degradation. It was also shown that the formulation has strong influence on stability of tested compounds. Forced degradation studies demonstrated the stability-indicating power of the method and can be used to assess the stability of paracetamol and potassium sorbate in oral liquid formulations.
Abstract
Baricitinib (BRT) is a drug substance with potent anti-inflammatory activity indicated in rheumatoid arthritis, atopic dermatitis, severe alopecia areata and recently for the treatment of Covid-19. Process impurities of the drug during its formulation are quite known, however studies regarding its degradation products (DPs) under stress conditions are limited. In this study, the drug was subjected to forced degradation under various degradation conditions, including acidic hydrolysis, alkaline hydrolysis, oxidative and thermal, to determine its inherent stability. To this purpose, a novel HPLC method was developed for the determination of degradation impurities of BRT. Alkaline hydrolysis test showed a selectivity towards breaking C–C bonds. This resulted to five DPs formed by chain scission reactions occurred at the pyrrolo-pyrimidine group between C6–C10 and C8–C9. Also, the ethylsulfonyl-azetidin-ylidene group was subjected to C–C bond cleavage at C12–C15 and C16–C18. Degradation products were further characterized with the use of liquid chromatography quadrupole time of flight tandem mass spectrometry (LC-Q-TOF-MS/MS).
Abstract
A gradient high-performance liquid chromatography (HPLC) method has been developed to determine the concentrations of latanoprost (LP) and latanoprost free acid (LPA) in aqueous solutions. It is novel due to a combination of its simplicity, speed, and detection capability in aqueous solutions for both active drug (LPA) and prodrug (LP). This method is applicable for the research and development of novel drug delivery devices and quality control assays for experimental and commercial laboratory settings, as it allows for a high sample throughput. Samples were chromatographed across a C18 + 2.7 µm 4.6 × 7.5 mm reversed-phase column with gradient elution using a mobile phase of aqueous acetic acid (pH 3.1) and acetonitrile with 0.1% acetic acid. UV spectrophotometry was used to monitor the eluents at 210 nm. Drug concentrations from 1.0 to 150 μg mL−1 were tested, with good linearity observed across the range. LPA had a signature peak at approximately 4.82 min (SD < 0.08) and LP at 9.27 min (SD < 0.07). For both drug and pro-drug, LOD and LOQ were 1.0 and 2.5 μg mL−1, respectively. This assay which accurately measures both prodrug and drug in a single injection, has significant applicability in determining the release kinetics of novel LP drug delivery systems.
The rice plant is sensitive to soil salinity. Calcium (Ca) acts as an ameliorative agent that helps plants induce salt tolerance. This study was carried out with a comparison of the ameliorative effect of calcium on salt-stressed rice seedlings, the determination of the role of salt-responsive protein groups, and the analysis of their genetic expressions in 21-day-old rice seedlings of ten locally cultivable varieties of West Bengal. For this study, 15-day-old seedlings were treated with 200 mM of sodium chloride (NaCl) solutions along with 10 mM of calcium sulfate (CaSO4) treatment. The determination of the relationship between the salt-responsive proteins and the analysis of the gene expression of those corresponding proteins were not carried out earlier on the selected ten locally cultivable rice varieties of West Bengal. The NaCl crystals were visible on the abaxial leaf surface of salt-stressed rice seedlings. The superoxide dismutase activity was increased in rice varieties, and a similar result was also expressed with calcium treatment. The fourier transform infrared spectroscopy-attenuated total reflection spectral result gave strong evidence for the presence of several salt-tolerant proteins and their genetic expression. STRING database results have suggested that the calcium treatment, coupled with the expression of the CBL4 protein, has regulated the P5CR protein of proline biosynthesis for better salt tolerance and osmotic protection. The quantitative real-time polymerase chain reaction and SDS-PAGE gel electrophoresis analysis showed that salt-tolerant varieties, Chinsurah_nona_1, and Jarava had high calcium signaling mechanisms and osmo-protection abilities.
Abstract
The advection-convection models (ACM) have practical applications in the investigation of separation processes, where mass (heat) is transferred by convection and diffusion (dispersion) along mass/heat exchanger, eq. adsorption, chromatography column, tubular reactor, etc. The ACM consists of nonlinear partial differential equations which can be solved only with numerical methods. In the article, a comparison of the volume method (VM) and orthogonal collocation on finite elements (OCFE) is presented in terms of their reliability, accuracy of calculations, and speed of calculation. The OCFE proved to be more robust than VM.
The linear ACM model for the chromatography column has an analytical solution in the form of the equation for the number of theoretical plates (N). This equation is often applied in the interpretation and evaluation of model parameters. However, the versions of N equation published in the literature are not correct. The error can lead to significant imprecision for specific cases. Here, in the paper, the revised equations are presented and discussed for the most frequently used chromatography column models.
Abstract
This study attempted to optimize pectin extraction from queen pineapple (Qp) peels using microwave-assisted method. A three-factor factorial experimental design was employed to test the interaction of moisture content of pineapple peel, pH of the citric acid solution and extraction time. The three-way interaction among the factors has a significant effect on pectin recovery. Two-way interaction between moisture content and pH level, as well as pH level and extraction time caused significant difference in the pectin recovery. Pectin recovery increases with lower moisture content while longer extraction time does not significantly increase pectin recovery. The optimum combination of the parameters is 12% moisture content, pH level 2 of the citric acid solution, and extraction duration of 2 min, which yielded 1.01 ± 0.01% pectin recovery. This is lower than the results from previous studies on pineapple with 3.88–13.06% pectin recovery using acid extraction method. Hence further optimization is recommended.
Abstract
Plant protection products (PPP), crucial for agricultural production, are experiencing increased global demand, particularly with the growing need for food production. To meet this demand, robust analytical methods are essential for confirming the presence and determining active substance concentrations in PPP. This study introduces an analytical method utilizing high-performance liquid chromatography with a diode array detector (HPLC-DAD) for determination of acetamiprid in water-soluble powder formulations. The method, validated according to SANCO/3030/99 rev.5, demonstrated exhibited adequate accuracy and precision, with repeatability expressed as the ratio of the standard deviation (% RSD) to the relative standard deviation (% RSDr) being lower than 1. Recoveries for the active substance at concentrations above 10% ranged from 97% to 103%. The developed method is also characterized by suitable linearity, confirmed by a correlation coefficient >0.99. Specific chromatographic profiles were generated, and acetamiprid content in 180 formulations was analyzed, including reference products. The developed method aligns with “green chemistry” principles, minimizing solvent use and emphasizing energy efficiency. Overall, it offers a comprehensive approach for qualitative and quantitative analysis, ensuring the reliability of PPP quality control.
Pilóta nélküli légi járművek alkalmazása a vizes élőhelyek modern felmérésében
Application of unmanned aerial vehicles as modern tools for wetland monitoring
A vizes élőhelyek a vízi és a szárazföldi ökoszisztémák között elhelyezkedő, igen változatos, és általában nehezen lehatárolható területek. Kiemelt jelentőségük annak köszönhető, hogy bár csak a globális szárazföldi területek mintegy 6–7%-át borítják, kulcsfontosságú szerepet játszanak az éghajlat szabályozásában, a vizes ökoszisztémák biodiverzitásának és hidrológiai viszonyainak fenntartásában, valamint számos további ökológiai és társadalmi funkciót is szolgáltatnak, beleértve az árvízvédelmi, víztisztítási, szén-dioxid-tárolási, élőhelytámogatási és kulturális, rekreációs előnyöket. A vizes élőhelyek azonban mind természetes, mind antropogén hatások következtében térben és időben is dinamikusan változnak, ezért védelmük és megfigyelésük napjainkra igen fontos kutatási területté nőtte ki magát. A műholdas távérzékelés nagyobb területek egyidejű megfigyelését teszi lehetővé, azonban érzékeny a felhőzetre és a légköri hatásokra, bizonytalanságot okozva ezzel az eredményekben. A hagyományos monitoring technológiák mellett a pilóta nélküli légi járművek térnyerése egyre kifejezettebb, köszönhetően rugalmasságának, hatékonyságának és alacsony költségének, miközben nagy térbeli és időbeli felbontású, szisztematikus adatszolgáltatásra képes. Tanulmányunk a pilóta nélküli légi járművek alkalmazási lehetőségeibe nyújt betekintést a vizes élőhelyek felmérésében, valamint áttekinti és összehasonlítja az egyéb távérzékelés technológiák alkalmazhatóságát ezen területek megfigyelésében. Célja, hogy elősegítse a dróntechnológia további terjedését és széles körű alkalmazását a vizes élőhelyek monitorozásában.
Abstract
In this work, an assessment of effective solvents and extraction methods was carried out to recover the bioactive compounds from hawthorn fruit (Crataegus monogyna Jacq.). Extractions assisted by heat, microwave, and ultrasound were carried out using various organic solvents (methanol, ethanol, and isopropanol). pH differential, Folin–Ciocalteu's, and aluminum chloride methods were used to determine total monomeric anthocyanin (TMA), total phenolic compound (TPC), and total flavonoid content (TFC), consecutively. Ferric Reducing Antioxidant Power (FRAP), 2,2-Diphenyl-1-picrylhydrazyl Hydrate (DPPH), and 2,2′- azino- bis (3-ethylbenzothiazoline-6- sulfonic acid) (ABTS) assays were used to measure the antioxidant activity (AA) of the extracts. The outputs revealed that extraction methods and solvents significantly affect anthocyanin concentration, TPC, TFC, AA, and color values of hawthorn fruit extracts. Due to the highest recovered TMA (0.152 ± 0.002 mg ECy3Gl/g of dry weight), TPC (49.14 ± 0.38 mg gallic acid equivalents/g of dry weight), and TFC (18.38 ± 0.19 mg quercetin equivalents/g of dry weight) contents, the ultrasonic-assisted extraction is superior to heat and microwave-assisted extractions. Accordingly, it was also observed that the methanol solvent is more profound than ethanol and isopropanol. Further, the bioactive compounds' content and the extracts' antioxidant activity are shown to be highly correlated. Thus, hawthorn extracts are considered to have antioxidant properties because of their concentrated bioactive compounds.
Abstract
Venetoclax is the first oral Bcl-2 inhibitor with high affinity targeting tumor cell apoptosis mechanism. In this study we developed a simple, sensitive and reliable LC–MS/MS method to determine venetoclax in children's hemolytic or lipemic samples. The method utilized an electrospray ion source and operated in multiple reaction monitoring mode. Venetoclax-d8 was used as an internal standard. Plasma samples were precipitated by acetonitrile containing 10% dimethyl sulfoxide and were separated by a Hypersil GOLD column (2.1 mm × 150 mm, 5 μm). The mobile phase consisted of acetonitrile-2 mM ammonium acetate (30:70, v/v) containing 0.4% formic acid. The quantification for venetoclax and venetoclax-d8 were m/z 868.1 → 636.1, m/z 876.1 → 644.1, respectively. The linear range was 10–2,000 ng mL−1 for venetoclax. The matrix in normal plasma, hemolytic or lipemic plasma had no significant effect on the detection results. The specificity, recovery and stability also met the acceptance criteria of guiding principles for the validation of biological sample quantitative analysis presented in the Chinese Pharmacopoeia (2015). As a result, this method is particularly suitable for determining venetoclax in hemolytic or lipemic samples from children with acute myeloid leukemia. The method, with the application of monitoring drug concentrations in pediatric patients, was successful.
Abstract
Due to the relative independence from the operational parameters, the linear retention indices (LRIs) are useful tool in gas chromatography-mass spectrometry (GC-MS) qualitative analysis. The aim of the current study was to develop a multiple linear regression (MLR) model for the prediction of LRIs as a function of selected molecular descriptors. Liquid injection GC-MS was used for the analysis of Essential oils (Rose, Lavender and Peppermint) separating the ingredients by a semi-standard non-polar stationary phase. As a result, a sum of 103 compounds were identified and their experimental LRIs were derived relying on reference measurements of a standard mixture of n-alkanes (from C8 to C20). As a next step, a set of molecular descriptors was generated for the distinguished chemical structures. Further, a stepwise MLR was applied for the selection of the significant descriptors (variables) which can be used to predict the LRIs. From an exploit set of over 2000 molecular descriptors, it was found that only 16 can be regarded as significant and independent variables. At this point split validation was applied: the identified compounds were randomly divided into training (85%) and validation (15%) sets. The training set (87 compounds) was used to derive two MLR models by applying i) the ‘enter’ algorithm (R 2 = 0.9960, RMSЕ = 17) and ii) the ‘stepwise’ one (R 2 = 0.9958, RMSЕ = 17). The predictive power was assessed by the validation set (16 compounds) as follows i) q2 F1 = 0.9896, RMSE = 25 and ii) q2 F1 = 0.9886, RMSE = 26, respectively. The adequateness of both regression approaches was further evaluated. Newly developed headspace-solid phase microextraction (HS-SPME) procedures in combination with GC-MS were used for an alternative analysis of the studied Essential oils. Twelve additional compounds, not previously detected by the liquid sample introduction mode of analysis, were identified for which the values of the significant descriptors were within the working range of the developed MLRs. For the last compounds, the LRIs were calculated and the experimental data was used as an external set for assessment of the regression models. The predictive power for both regression approaches was assessed as follows: Enter RMSE = 41, q2 F2 = 0.9503 and Stepwise RMSE = 40, q2 F2 = 0.9521.
Abstract
Monitoring benzoylphenylureas (BPUs) residues in ready-to-eat vegetables is of great interest for an adequate assessment of human pesticide exposure. A rapid, inexpensive, simple, and effective method for determining 8 BPUs insecticides in tomatoes and cucumbers was developed and validated. Vortex-assisted liquid-liquid extraction (VA-LLE) followed by dispersive solid-phase extraction (d-SPE) using graphitized carbon black (GCB) for cleanup was used before LC-MS/MS analysis. Different parameters were optimized, including the type and volume of extractants, vortex time, and the type and amount of adsorbents used for cleanup. The evaluation showed that the method has excellent linearity (R 2 ≥ 0.994). The recovered 8 BPUs insecticides from spiked tomato and cucumber samples at 0.01, 0.05, and 0.25 mg kg−1 ranged from 83.2 to 105.2%, with RSD of 4.9–14.6%. The limits of quantitation (LOQs) were 0.0025 mg kg−1 (0.005 mg kg−1 for lufenuron). Within-day repeatability ranged from 3.9 to 13.9%, while between-day repeatability ranged from 8.9% to 17.7%. The optimized method was used to analyze 100 samples of tomatoes and cucumbers marketed in Saudi Arabia.
A hazai genetikai talajosztályozás megújításának szükségessége - 1.
A nevezéktan és a struktúra korrekcióra szoruló elemeinek azonosítása
The necessity of the renewal of the Hungarian genetic soil classification system - 1.
Identification of the elements of the nomenclature and structure to be corrected
A tanulmány a magyar genetikai osztályozás sok szempontból kritizált rendszerének következetlenségeit, illetve ellentmondásait elemzi azzal a szándékkal, hogy a rendszer fő jellemzőinek: a talajtaxonok elnevezésének és tartalmának megőrzése mellett szakmai párbeszédet indítson a hibák kijavításának lehetőségéről és a rendszer megújításáról.
Rámutattunk a nevében és koncepciójában genetikus, szerkezetében hierarchikus osztályozási rendszer hibrid jellegére: arra, hogy a fő genetikus szempont csak a főtípusok aggregációs szintjén érvényesül maradéktalanul, míg a típusoknál már mintegy egyharmad arányban diagnosztikus szempontok jelentik az elkülönítés alapját. Alsóbb hierarchiaszinteken (altípus, változat) pedig csaknem tisztán diagnosztikus az osztályozás. Listába rendeztük azokat a problémás típus, altípus és változati elnevezéseket, amelyek több hierarchiaszinten azonos névvel, és esetleg eltérő tartalommal fordulnak elő, illetve azonos hierarchiaszinten, de eltérő definíciókkal szerepelnek, vagy éppen szinonímnak tekinthetők, az eltérő elnevezés mögött rejlő azonos tartalom miatt. A vitacikk szándéka, hogy a kiszűrt hibák, következetlenségek széleskörű szakmai egyeztetést követően javításra kerüljenek.
Abstract
In this study, a multivariate optimization strategy was used to develop and validate a simple, rapid, accurate, cost-effective, and stability-indicative RP-HPLC analytical method for quantifying hydroxychloroquine sulphate (HCQ) in coated tablets. The validation conditions involved isocratic elution mode, using a mixture of buffer solution at pH 2.2 and methanol (74:26, v/v) as the mobile phase, an Agilent® reverse phase column, model Zorbax Eclipse Plus C18 (250 cm × 4.6 mm × 5 μm), a flow rate of 1.3 mL min−1, column temperature 40 °C and detection at 343 nm. The method showed linearity in the range of 4–44 μg mL−1, with a correlation coefficient (R) of 0.9998. Recovery obtained average values of between 99.71 and 100.84% and precision with average RSD values of <2%. The robustness demonstrated by assessing the effect of seven variables (pH of the mobile phase buffer; percentage of methanol; filter brand; mobile phase flow rate; wavelength; column temperature and sample agitation time), with effect values for each variable lower than the calculated value of s√2 (1.43), showed that none of these factors had a significant influence on the analytical response. The method was applied to samples of the reference medicine Plaquinol® 400 mg and similar Reuquinol 400 mg, nomenclature established by the National Health Surveillance Agency (Anvisa), law no. 978 of 10 February 1999, purchased from local pharmacies. Results showed advantages and benefits in relation to the official method and those reported in the literature. The application of the multivariate strategy, the choice of methanol, in a lower proportion in the organic phase, due to its low toxicity, economy and easier availability compared to acetonitrile, and the other organic solvents used was a promising and important alternative for the analytical method. Furthermore, the use of reversed stationary phase, common in quality control laboratories, provided an analyte retention time of 4.595 min, demonstrating good performance and speed in routine analyses.
Abstract
An ion chromatographic method and its application have been described to quantify nine cationic components (lithium, sodium, ammonium, methylammonium, potassium, magnesium, calcium, strontium, and barium) in pyrotechnics (firecracker and firework) samples. The samples in this study were purchased from local shops in Ternate City, North Maluku. The method performed a mixed eluent with 4 mM HNO3 and 0.015 mM Na2EDTA, combined with a Metrosep C4-150/4.0 separation column for all quantifications. Excellent chromatograms were achieved, and the nine cationic components were eluted in less than 18 min. The calibration graphs of the quantifications were linear in the range of 1.25–37.5 mg L−1. The detection limit (LOD) at S/N = 3 was below 0.098 ppm (mg L−1). This method was applied to the pre-blast and post-blast residues of pyrotechnics samples, and the simultaneous quantification of the nine cationic components in these samples was achieved with satisfactory results.
A talajspektrális könyvtárak nemzetközi jelentősége és hazai megalapozása
The international importance and national establishment of soil spectral libraries
Napjainkban soha nem látott igény mutatkozik megfelelő mennyiségű és minőségű talajadatra és információra. Spektroszkópiai technológiák a hagyományos laboratóriumi módszerekkel együttesen, párhuzamosan alkalmazva lehetőséget kínálnak a talajfelvételezés idő- és költséghatékonyabbá, valamint környezetkímélőbbé tételére. Jelen munkában lokális, regionális és globális léptékű talajspektrális könyvtárak bemutatása mellett az első országos szintű, az Agrártechnológiai Nemzeti Laboratórium projekt keretében kidolgozásra kerülő, Magyarország talajtani változatosságát reprezentáló spektrális adatbázis létrehozásának koncepcióját mutatjuk be. A spektrális könyvtárak olyan speciális talajadatbázisoknak tekinthetőek, melyek tartalmazzák egy adott terület talajait reprezentáló talajminták hagyományos laboratóriumi módszerrel meghatározott paramétereit, valamint spektroszkópiai módszerrel rögzített spektrumait. A spektrális könyvtárakban tárolt adatok alapján elvégzett, spektroszkópiai kalibrációkra alapozott talajparaméter becslési eljárások lehetőséget kínálnak az adatbázisban szereplő talajminták fizikai-kémiai-ásványtani tulajdonságaihoz hasonló minták paramétereinek spektrális alapú megbízható megbecsléséhez. A hazai spektrális könyvtár alappillérét a Talajvédelmi Információs és Monitoring (TIM) rendszer mintavételezés kezdeti évében (1992-ben) gyűjtött, talajok genetikai szintjeiből vett talajmintákról felvett spektrumokra építjük. A spektrális adatbázist a középső-infravörös (middle-infrared, MIR), valamint a látható- és közeli infravörös (visible and near-infrared, VIS-NIR) tartományban, a Global Soil Laboratory Network (GLOSOLAN) iránymutatásai alapján rögzített spektrális adatokra építjük. A folyamatosan bővülő spektrális könyvtár, és az erre az adatbázisra épülő talajtulajdonság-becslő eljárás lehetőséget fog kínálni számos fizikai és kémiai paraméterének megbízható meghatározására, ezzel (számottevő többletköltség nélkül) nyújt lehetőséget a jelenlegi laboratóriumi kapacitás növelésére.
Abstract
Soil cultivation techniques can change the physical properties of soil and have the potential to influence the growth and productivity of crops. In the 2022 season, a research study was carried out on Gypsfreous soil in the College of Agriculture fields at Tikrit University. The purpose of the study was to investigate how the physical properties of the soil are influenced by three different plow types and varying plowing speeds. The study was planned using split plots within a Complete Randomized Blocks Design, with three types of plows (moldboard plow, disc plow, and chisel plow) and three tractor speeds (3.8, 5.8, and 7.6 km h−1) as the experimental treatments.
The experiment's findings indicated that the moldboard plow resulted in a greater reduction in bulk density compared to the disc plow. Consequently, the soil's bulk density decreased, and the percentage of porosity increased. On the other hand, the chisel plow had the lowest soil-specific resistance value and the highest soil volume disturbed value. The speed of operation above 3.8 km h−1 proved to be the most effective in reducing bulk soil density, increasing soil porosity, and reducing specific soil resistance. However, at a speed of 7.6 km h−1, the soil volume disturbed was significantly higher than at other speeds. Additionally, the experiment's findings demonstrated that the moldboard plow, operating at a speed of 3.8 km h−1, was significantly more effective than other methods in decreasing the soil's bulk density, increasing the porosity percentage, and reducing the specific soil resistance. Conversely, the chisel plow, working at a speed of 7.6 km h−1, had a significant advantage in achieving the highest value for the volume of soil disturbed.
Abstract
An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of nobiletin and tangeretin in rat plasma, and the plasma was processed by a simple liquid-liquid extraction method with ethyl acetate. The chromatographic column was UPLC HSS T3 (50 × 2.1 mm, 1.7 μm), the mobile phase was acetonitrile-water (containing 0.1% formic acid). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, nobiletin m/z 403.29 → 373.14 (cone voltage 22v, collision voltage 28v), tangeretin m/z 373.28 → 343.17 (cone voltage 20v, collision voltage 28V), tangeretin m/z 373.28 → 343.17 (cone voltage 20V, collision voltage 28V) and internal standard vitexin m/z 433.14 → 313.03 (cone voltage 32v, collision voltage 26v). The pharmacokinetics of nobiletin and tangeretin were evaluated in rats. The established UPLC-MS/MS method in the range of 2–2,000 ng mL−1 was successfully applied to the pharmacokinetics, and the calculated bioavailability of nobiletin and tangeretin was 63.9 and 46.1%, respectively.
Abstract
Based on chromatographic fingerprinting combined with quantitative analysis on characteristic chemical constituents as well as hierarchical cluster analysis, an easy and sensitive approach utilizing high performance liquid chromatography (HPLC) was developed for the identification and quality evaluation of Rutongshu oral liquid (ROL). What is more, nontargeted metabolomic analysis was conducted to gain a global view in terms of its chemical profile. In this study, 16 peaks from different batches (S1–S10) of ROL samples produced by Taihe Hospital of Chinese Medicine were selected as common peaks for the evaluation of their similarity whose values of all tested 10 batches exceeded 0.90 when compared with the control fingerprints. Meanwhile, simultaneous quantification of five markers in the oral solution, including albiflorin, paeoniflorin, chlorogenic acid, quercetin and ferulic acid was performed, and standard curves established for respective reference substances showed good regression in the linear range (r 2 > 0.999) with recoveries in the range of 98.96–102.35%. The ultra-high performance liquid chromatography (UHPLC) combined with Orbitrap Exploris 120 mass spectrometer resulted in 88 identified compounds. The results of validation showed that the established method was reproducible, precise and stable. This study offers an effective, dependable and useful approach for the systematic evaluation of the hospital formulation ROL.
Abstract
Hydrochlorothiazide has been utilized clinically for the past half-century, which is popularly known as a “water pill” as it produces increased urine output. The advancement of bioanalytical methods brought a dynamic field with exciting opportunities for future research. The current review emphasis the bioanalytical methods employed for the quantitative estimation of Hydrochlorothiazide as monotherapy and its popularly used combinational medications available from 1956 to till date. A fixed dose of 25 mg of hydrochlorothiazide with 43 combinational medications is currently available in the market and these combinations are widely employed in the treatment of hypertensive people; those whose blood pressure does not respond effectively to monotherapy of hydrochlorothiazide and also for the treatment of edema (excess fluid in the body) caused by illness such as heart failure, liver problems, and renal disease. It has been convincingly demonstrated that the combination of any two antihypertensive medications belonging to different groups of the same category, significantly lowers blood pressure, in comparison with the effect produced by increasing the dose of a single medicament. Among the various analytical techniques employed for the estimation of Hydrochlorothiazide, the review portrays that hyphenated technique, in specific liquid chromatography coupled with mass spectroscopy was widely employed. The validation parameters namely linearity, LOD, LOQ for individual drug and their combinations, were successfully calibrated. The effectiveness of analytical approaches was evaluated and enhanced for chemical factors. The involvement of green chemistry in the optimized methods for the evaluation of Hydrochlorothiazide for the future development, are suggested.
Abstract
This review focuses on monosodium glutamate which proclaims the fifth taste as “Umami”. Monosodium glutamate imparts a deep, meaty, umami flavour to foods. Asian cuisine frequently uses this flavouring, just as in the processed items produced across the United States and Europe. This article dealt with a detailed discussion of physicochemical features, pharmacological actions, and different reported analytical methodologies for the estimation of monosodium glutamate. Monosodium glutamate is analyzed using a variety of techniques, including spectroscopy, chromatography, electrochemistry, electrophoresis, chemometrics, flow injection analysis, and biosensors. According to results of comparative research of analytical methodologies, high performance liquid chromatography (HPLC) is most widely used method for analyzing monosodium glutamate which surpasses the gas chromatographic (GC) approach. All of the reported methods are accurate, precise, cost-effective, and sensitive. The European Union defined monosodium glutamate as a food additive that is permitted in some foods, but is subject to quantitative limits. Consequently, this study provides the analyst with an accessible path to quantifying monosodium glutamate's content for use in the food and pharmaceutical industries.
Abstract
A straightforward, dependable, and quick RP-LC method for the analysis of abiraterone acetate in its dose form and human urine has been devised. With DAD detection, sensitivity was reported to be high. The LOD and LOQ of the procedure were deemed adequate. The suggested approach was exhaustively validated in accordance with ICH requirements, and the findings demonstrated that it was exact, accurate, selective, and sensitive for the analysis of this pharmaceutical. The chromatographic separation was realized using a X-Terra RP-18 (150 × 4.60 mm i.d. × 5 μm) column and a UV detector set at 255 and 267 nm. In addition, pK a values were calculated based on the relationship between the retention factor and the pH of the mobile phase. The influence of the composition of the mobile phase on the ionization constant was investigated by measuring the pK a at various acetonitrile–water combinations ranging from 50 to 70% (v/v).
Abstract
Lenalidomide is a drug that has immune-modulating, anti-angiogenic, and anti-inflammatory properties. In this study, we developed green HPLC and spectrophotometric methods to determine the concentration of lenalidomide in pure and pharmaceutical formulations. In the HPLC method, 10 mM potassium dihydrogen phosphate solution (pH: 2.0) and ethanol (50:50, V/V) were used as mobile phases, isocratic elution was applied at a flow rate of 1.0 mL min−1 and detection was made at 304 nm. In the spectrophotometric method, the spectral patterns of standard solutions in different solvents were comprehensively examined, the best spectra were obtained with ultrapure water, and a wavelength of 304 nm was selected for detection. Both methods have been validated according to ICH guidelines for various parameters. Correlation coefficients greater than 0.999 were determined for both methods in the concentration range of 5–30 μg mL−1. The developed methods were applied to commercial formulations, and comparisons of the results were made using the Student (t) test for means and the Fischer (F) test for standard deviations. No statistically significant difference was observed between the methods. The greenness evaluation of these methods was carried out using AGREE software. The developed methods are proposed as excellent environmental and operator-friendly alternatives for the quantification of Lenalidomide in pharmaceutical formulations.
Abstract
“Feed the global population and regenerate the planet.”
The conditions necessary for the implementation of the above commonly used slogan did not exist 10–15 years ago. We did not have access to the information and databases that would have allowed us to increase yields for the purpose of feeding the growing population. While increasingly meeting sustainability requirements and regenerating the Earth. Anthropocentrism, the belief that humans are superior to everything else, benefits humans by exploiting human greed and ignorance, which is a dead end for both individuals and societies. Only humans can ignore the dynamic equilibrium processes of nature and disregard the consequences that adversely affect future generations. Ecocentric agricultural practices have several prerequisites. It is important for the academic sphere to recognize its significance. Another fundamental challenge is the continuous monitoring of the production unit and its close and distant environment for the purpose of decision preparation using Big Data. The Internet of Things (IoT) is a global infrastructure that represents the network of physical (sensors) and virtual (reality) “things” through interoperable communication protocols. This allows devices to connect and communicate using cloud computing and artificial intelligence, contributing to the integrated optimization of the production system and its environment, considering ecocentric perspectives. This brings us closer to the self-decision-making capability of artificial intelligence, the practice of machine-to-machine (M2M) interaction, where human involvement in decision-making is increasingly marginalized. The IoT enables the fusion of information provided by deployed wireless sensors, data-gathering mobile robots, drones, and satellites to explore complex ecological relationships in local and global dimensions. Its significance lies, for example, in the prediction of plant protection. The paper introduces small smart data logger robots, including the Unmanned Ground Vehicles (robots) developed by the research team. These can replace sensors deployed in the Wireless Sensor Net (WSN).
Abstract
Hungary is a Central European country that is rich in medicinal and aromatic wild plant species; in rural livelihoods, the collection, use, process, and trade of these plants are traditionally important contributors. However, due to several recent changes touching the sector, the natural ecosystems, biodiversity, and collectors - who generally belong to poorer social groups – are affected negatively.
The paper aims to introduce the Hungarian herbal sector from a holistic perspective, including its economic, environmental, and human dimensions, with a particular focus on sustainability. In this context, the purpose of the article is to discover this field as comprehensibly as possible and present it from both theoretical and practical aspects. Another objective is to collect the best practices and feasible solutions from the field in connection with promoting a harmonious, as well as economically prosperous relationship between nature and local people. This integrated approach helps show the industry's strengths and advantages, as well as its weaknesses and challenges. Based on the findings, the paper attempts also to propose some recommendations for the future.
„Két lábbal a földön, avagy miként próbál a talajtan válaszokat adni a globális kihívásokra”
Beszámoló a HUN-REN ATK Talajtani Intézetének Magyar Tudomány Ünnepe előadónapjáról
Abstract
Peanut butter and yoghurt are targeted for adulteration intended at consumer deception. This study aimed to fingerprint and detect peanut butter and yoghurt adulteration with cassava flour and starch using Near Infrared Spectroscopy (NIRS) in a quasi-experimental approach. Ingredients for laboratory sample preparation were obtained from the Kumasi Metropolis. Peanut butter was adulterated at 1, 3, 5, 10, 15, 20% w/w and yoghurt at 0.25, 0.5, 1, 3, 5, 10, 15, 20, 25, 45, 50% w/w. Selected concentrations mimicked practices on the market. Marketed products were randomly sampled from six markets in the Kumasi Metropolis to validate the study models. Samples were scanned with a hand-held NIRS in triplicates. Chemometric (Principal Component Analysis (PCA), Linear Discriminant Analysis (LDA) and Partial Least Square Regression (PLSR) models) statistical methods were employed to develop classification and prediction models. Peaks with spectral bands such as 1050 , 1200 and 1450 nm were observed for peanut butter and 990–1100 nm, 1100–1200 nm and 1300–1408 nm were observed for yoghurt in the NIR spectrum. Some yoghurt brands were suspected of containing cassava starch, while Peanut butter from the different markets differed based on classification models. Cassava flour and starch concentrations were quantitatively predicted by PLSR with an R2 CV of 0.98 and an error of 0.9 g/100 g (low error).
A talaj katabolikus aktivitás mintázatának elemzése mikrorespirációs (MicroResp™) módszerrel
Analysis of soil catabolic activity patterns by micro-respiration (MicroResp™)
A talaj mikrobiális közösségének funkcionális diverzitása a talaj ökoszisztéma szolgáltatások jelentős részéhez hozzájárul, sok esetben meghatározó jelentőségű. Többféle kísérleti és elméleti megközelítés közül a katabolikus aktivitás-mintázat mikrorespirációs – MicroResp™ – módszerrel történő megközelítését mutatjuk be. A módszer a régebbről ismert szubsztrát-indukált respiráció több-szubsztrátos, mikrotiter lemez alapú kiterjesztése, amivel a talaj mikroba-közösség in-situ közösségi-szintű fiziológiai mintázata határozható meg. Mivel az egyes mikroorganizmusok szubsztrát-hasznosítása eltérő, a mikroba-közösség aktuális összetételétől, abundanciájától függően változó a szubsztrát hasznosítási mintázat egy-egy talajminta esetében. Az alkalmazott szubsztrátok köre tetszőleges, rendszerint egyszerű cukrok, aminosavak, aminok, karbonsavak. A módszer gyors, érzékeny, megbízható, ezért alkalmazása tervezett kísérletekben és talajmonitoring programokban egyaránt javasolható.
Abstract
The soaking step of dry pulse products' – e.g. chickpeas' – food processing is a time consuming process. Soaking time can be significantly reduced by ultrasonic treatment or using higher processing temperatures. The effect of ultrasonic treatment can be investigated by examining the soaking water characteristics. Ultrasound-assisted soaking of chickpeas was performed at 25, 35 and 45 °C, respectively. Additionally, control samples were also prepared without ultrasonic treatment at the same temperatures. The dynamics of the fitted curve clearly shows the relationship namely the higher the treatment temperature, the faster the hydration of the raw material for both untreated and treated groups. In contrast to control group, swelling rate of 2.00 – except the group 45 °C – is not achieved during ultrasound-assisted soaking. In case of treated group, the swelling rate was about 1.90 for all temperatures applied. The ANOVA test shows that the color of the ultrasonically treated samples was significantly different compared to the control (F (5;12) = 207.86; P < 0.001). Average dry matter content and °Brix value were significantly higher in the ultrasound treated group compared to the control in case of all temperatures. This may indicate the destructive effect of ultrasound, which may cause more components to dissolve out of the raw material by the end of the soaking process.
Abstract
The objective of our work was to analyze the differences between four nut pastes, which were the following: walnut, peanut, pistachio, and tahini (sesame). The process technology of them is unknown, however, all the products contain 100% nut without any additives or flavoring.
The paste samples were measured at 25 ± 0.2 °C. The apparent viscosity at a 10 1/s shear rate during flow curve recording, and the dynamic viscosity at a constant 20 1/s shear rate was determined by viscosity measurement with the use of the MCR302 modular compact rheometer. The L*a*b* color components were determined by ColorLite sph850 spectrometer, finally, the particle sizes and shapes of the samples were analyzed by the high-speed image analysis instrument QICPIC.
The apparent viscosity and the average dynamic viscosity values of the four nut pastes were significantly different from each other. Differences were found between each paste according to the L*a*b* parameters. The complex structures of the particles are detailed and measurable, whereby the lengths and diameters of the particles can reliably be determined and fine deviations between the samples are detected. The sphericity decreases slightly with increasing particle size which means that bigger particles are more irregularly shaped.
Abstract
In this study, two different ethanol-based RP-HPLC methods for assay and quantification of rivaroxaban related substances in tablets were developed, based on green analytical chemistry (GAC) principles, using the design of experiments approach. The chromatographic separation was performed on X-Bridge C18 column (250 × 4.6 mm, 5 µm particle size), using isocratic elution with ethanol : water (35:65, % v/v) for the assay and gradient elution with ethanol/water mobile phase, for related substances, with a flow rate of 1.0 mL min−1. The gradient method was optimized for the separation of three specified impurities (impurity G, impurity H, and impurity 14) and the selectivity was further confirmed using forced degradation studies. Both methods were validated in accordance with ICH guidelines. The robustness of the methods was confirmed with the Central Composite Face Design of Experiments. Analytical Eco-scale approach and AGREE metrics confirmed that both methods are in accordance with the GAC principles. The proposed ethanol-based RP-HPLC methods were applied for assay and determination of related substances in rivaroxaban 10 mg tablets obtained from three different manufacturers available on the Macedonian market.
Abstract
With growing attention to health and lifestyle changes, functional foods have become crucial and in demand. These foods are a rich source of probiotics and prebiotics, but most probiotic products are dairy-based, making them inappropriate for people with lactose intolerance or milk protein allergies. Nevertheless, egg white offers a viable substitute and is considered one of the best sources of functional proteins. As an alternative food matrix, they come highly recommended for those who are hypersensitive to dairy products or who follow a high-protein diet, such as athletes. In this context, egg-white drink with different carbohydrate sources, including monosaccharide (fructose) and oligosaccharide (fructooligosaccharide), was fermented by Lacticaseibacillus casei 01. After 24 h of fermentation, the total cell count was higher than 8 log10 CFU mL−1 thus, the egg white drink was suitable for L. casei 01 to grow. Additionally, the survival of L.casei 01, the pH value, and the rheological properties of fermented beverages within three weeks of refrigerated storage were also investigated. Throughout the storage period, the control samples exhibited considerably lower cell count and higher pH values compared to the samples with carbohydrate sources, also, samples containing the same carbohydrate source showed no noticeable changes. Viscosity measurements of the studied samples showed a shear thickening behaviour during the time.
Abstract
Tomato (Solanum lycopersicum L.) is grown worldwide in open fields and greenhouses in a range of climate conditions. Hedgerows are a type of agroforestry systems that monitors ecological and influence microclimate conditions. An experiment was conducted at the Soroksár experimental field of the Hungarian University of Agriculture and Life Sciences in 2022 to investigate the influence of hedgerow technology on tomato plant leaves, N, P, K, chlorophyll, and carotene mineral levels from different distances, Exposed sides W1-3m, W2-9m and W3-15m and Protected sides NP1-3m, NP2-9m and NP3-15m, meters from the hedgerow trees.
The results investigate potassium and carotene, as well as chlorophyll b levels, are less differed among the protected and exposed side of the hedgerows trees, while the others were impacted to a certain extent; nitrogen and chlorophyll content was generally higher on the exposed side regardless of variety, while in the case of phosphorus adverse effects were observed. Distance from the hedge showed similar patterns for all traits. The results will help to better understand the impact of alternate technologies on tomato production in open-field conditions.
Abstract
Polyphenols from agro-industrial waste particularly of fruit origin are a reliable source of antioxidants and antimicrobials that can be used as natural food additives. Organic solvents play an important role in extracting the polyphenols, however, inefficiency in exerting bioactivity and interference with the organoleptic properties are among the reasons that hinder their use as food additives. These problems can be alleviated by purification. In this study, the effect of resin types and elution solvent for purification of the apple pomace extracts on total phenolic content (TPC) and antioxidants were investigated. Crude ethanolic extracts were purified using amberlite resins (XAD7HP and FPX66) in a glass column (25 × 310 mm). The sorption flow rate was 2 Bed volume (BV) per hour, rinse 2 BV per hour, and desorption was 2 BV per hour. Final wash and regeneration were each done by 2 BV per hour. Polyphenol content and antioxidant capacity were quantified spectrophotometrically using Folin-Ciocalteu and Ferric reducing ability of plasma (FRAP) assays respectively. Polyphenol recovery was 50% in XAD7HP (Lowest) using ethanol and 69% in FPX66 (Highest) using acetone. For the case of FRAP recovery, 76% (Lowest) was observed in FPX66 using ethanol while 93% (Highest) was observed in XAD7HP using acetone. Conclusively, FPX66 is the ideal resin for the purification of apple pomace extracts for enhancing antioxidant activity compared to XAD7HP. Further, acetone seems to be a good desorption solvent compared to ethanol.
