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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
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.
Abstract
Garcinol, the main polyisoprenylated benzophenone present in Garcinia species. A simple, rapid, reliable high-performance thin-layer chromatography (HPTLC) technique has been developed for simultaneous detection and quantification of garcinol in three endemic Garcinia sp. of Assam, India. While G. mangostana and G. indica have garnered extensive recognition, these lesser-known species have not received proportionate level of scientific exploration, therefore has served as the subject of investigation. Chromatographic separation was achieved using pre-coated silica gel 60 F254 plates. The optimized mobile phase (Toluene-Ethyl acetate-Formic acid, 5:4:1V/V) at 276 nm produced well-defined and sharp peaks of garcinol, maintaining a constant R F value of 0.75. The regression equation demonstrated a linear relationship with a correlation coefficient of 0.9955. The method was validated in accordance with International Conference of Harmonization guidelines (ICH), encompassing assessments for precision, accuracy, repeatability and robustness, all of which yielded low percentage of relative standard deviation values, attesting to its excellent performance. The content of garcinol found in the extracts were in the range of 0.58–0.98% w/w. In secondary metabolite analysis, significant amount of phenols (26.06 ± 1.65–57.51 ± 2.62 gallic acid equivalent mg g−1), flavonoids (11.27 ± 1.06–21.09 ± 1.34 quercetin equivalent mg g−1) and ascorbic acid (3.56 ± 0.12–3.65 ± 0.11 mg/10 g) contents were detected in the extracts. Further, the extracts exhibited good anti-radical activity, which may be attributed to the presence of important secondary metabolites. Therefore, this research establishes the three endemic Garcinia sp. as promising source of garcinol. Additionally, the developed method can be applied for routine quality control analysis of herbal formulations containing garcinol.
Abstract
This study aims to predict drought periods affecting the Tokaj-Hegyalja wine region and the application of this in crop protection. The Tokaj-Hegyalja wine region is the only closed wine region in Hungary with a specific mesoclimate and a corresponding wine grape variety composition, in which climate change strongly threatens cultivation. The probability that a randomly selected day in the vegetation period will fall into a drought period in the future was estimated using the daily precipitation amount and daily maximum temperature data from the Hungarian Meteorological Service for the period 2002–2020. The Markov model, a relatively new mathematical method for the statistical investigation of weather phenomena, was used for this. Markov chains can, therefore, be a valuable tool for organizing integrated pest management. This can be used to plan irrigation, control fungal pathogens infecting the vines, and plan the success of a given vintage.
Abstract
In accordance with the International Coordinating Committee's recommendations, an acceptable UPLC-MS method is being developed for analyzing Relugolix stability under various stress scenarios. Stress conditions included exposure to 0.1 and 1 N acid, alkali, hydrolysis, peroxide, light, reduction, and heat. The mobile phase for this analysis was prepared by blending acetonitrile and a 0.1% orthophosphate solution in a 50:50 (v/v) ratio. A C18 Column with dimensions of 100 × 2.1 mm and a particle size of 1.7 µm was employed as the stationary phase. The wavelength at which detection was performed was 247 nm, and the flow rate was maintained stable at 0.5 mL min−1. Strong linearity was shown by this method across a concentration range of 1.25 μg mL−1 to 7.5 μg mL−1. The method's reliability was shown by ensuring all of the validation parameters fell within the acceptable range.
Furthermore, forced degradation studies were conducted using standard drugs. Different stress conditions led to the formation of degradation products, which were successfully separated from Relugolix using the C18 column in combination with an auto-purification mass spectrometer. Among the stress conditions, alkaline conditions showed a lower degradation rate. Interestingly, seven distinct types of degradation products were identified from the degradation studies under acid, alkali, hydrolysis, hydrogen peroxide, light, reduction, and thermal conditions. Remarkably, these seven degradation products have not been reported in previous literature, making this study the first to document their existence.
Abstract
The utilization of sea buckthorn pomace (SBP) is attracting growing attention since it is valuable industrial waste. This pomace can find usage as a functional ingredient of food because it contains bioactive, health-promoting components, but to our knowledge, few scientists have so far studied utilization of the antimicrobial activity of fruit pomace. The study aims are to broaden our knowledge of antioxidant and antimicrobial status of SBP by utilizing pomace as a functional apple juice ingredient and by monitoring the antioxidant capacity, the total polyphenol content and microbial changes that occur during the storage of juice samples. Our results of this study highlight that the importance of the utilization of SBP because the results reported here provide further evidence that SBP can contribute to increasing the content of valuable components in apple juice samples and inhibiting the growth of microorganisms during storage.
