Browse Our Chemical Engineering Journals
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 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.
Abstract
This study investigates the effect of 2% lactic acid and 2% ascorbic acid mixture on the quality parameters of red deer meat and beef. After treatment samples were stored at 4 ± 1 °C. The following meat quality parameters were evaluated: pH, color, and microbiological count on days 1, 7, 14, and 21. The results showed that at the end of the experiment, the pH of the treated samples was slightly higher than the non-treated samples, indicating that the lactic acid and ascorbic acid mixture had a mild acidifying effect on the meat. The color of the treated and non-treated samples did not show any significant difference. However, the microbiological count in the treated samples was lower than the non-treated samples. These findings suggest that an acid mixture could be used as a natural preservative to enhance the microbial safety of red deer meat and beef.
Abstract
This study focuses on the contribution of maturity stages and 1-methylcyclopropene (1-MCP) treatment to the quality of ‘Zebra’ apricot. Samples were harvested at mature-green, yellow and orange maturity stages. Fruit were treated with gaseous 1-MCP (24 h at 1 °C), followed by cold storage at 1 °C for 6 weeks. Non-destructive measurements were used to evaluate the quality changes of apricot during storage. The results showed that the maturity stages significantly affected the weight loss. The loss of weight increased rapidly for orange ripeness stage fruit, more than others during storage. Both maturity and 1-MCP affected the stiffness of apricot. The 1-MCP could delay the softening of fruit. The green and yellow maturity stages retained higher values in stiffness compared to orange. No significant difference in hue angle values was observed between 1-MCP treated and control fruit, however hue angle value decreased strongly in mature-green harvested fruit. The maturity stages and 1-MCP treatment had the effect on quality changes of apricot over storage. The maturity stage was an important factor contributing to the effectiveness of 1-MCP application as it was observed in slower softening after harvest.
Abstract
Besides their unique taste and texture, mushrooms are a promising source of important nutrients, including dietary fiber, amino acids, minerals, and vitamins. Fresh mushrooms, however, can only endure for a brief time, typically up to three days at ambient conditions. Different methods have been used to preserve mushrooms for a prolonged period, such as drying, cooking, frying, irradiation and fermentation. The objective of the current study is to investigate the effect of different pre-treatments and fermentation on physicochemical, textural, and microbial properties of oyster mushrooms. The fresh oyster mushroom was considered as control and 6 alternative pre-treatment methods were used as; blanching in water, steaming, oven cooking, microwave, High Hydrostatic Pressure and UV Light treatment. Moisture, pH, yield, color, texture, and microbiological analyses were performed on each pre-treatment group before and after fermentation. Our results showed that the quality attributes of oyster mushrooms were significantly affected by the usage of different pre-treatments.
Abstract
The presented study investigated the effects of edible coatings with concentration of 2%, 3% and 4% of starch (w/v) on the weight loss and firmness loss of green asparagus during 4 days of storage at room temperature (26 ± 2 °C, 65–70% RH). According to the results, the coated asparagus exhibited significantly slower deterioration rate than the uncoated control samples. This was indicated by the decrease in weight loss and increase in firmness (P < 0.05). After the storage period, the samples treated with 4% starch formula retained the highest quality. Furthermore, the assessment of asparagus quality throughout the storage period involved the use of the line laser scattering technique. Extracted parameters of laser scattering signal discriminated samples with linear discriminant analysis (LDA), in which the correct recognition rate of the treated groups was 75.26% and the storage time was 70.54%. This study showed the potential of laser scattering as a rapid, non-invasive, and practical optical method for assessing the quality of asparagus during storage.
Abstract
This study aimed to assess the effectiveness of two reverse osmosis membranes (RO99 and X20) plus one nanofiltration membrane (NF270) at concentrating hawthorn fruit and anise seed extracts. Extracting the anise was done using water at a temperature of 37 °C over a period of 100 min. For hawthorn, ethanol-water (56%) was used as the solvent and extraction occurred at 55 °C for 80 min. The transmembrane pressure (TMP), temperature, and recirculation flow rate of the membrane separation process were monitored and set at 35 bar, 30 °C, and 400 l/h respectively. Using a spectrophotometer, the quantification of valuable compounds was examined. After studying the flow levels, it was discovered that the X20 membrane had the tiniest alterations in permeability, followed by RO99 and NF270. Moreover, in terms of efficiency, the X-20 outperformed RO-99 and NF-270 membranes, where TPC was increased (20 and 18-fold) for anise seed and hawthorn fruit extracts respectively, and TFC was increased 8-fold for both of the extracts. While using NF-270, TPC was increased only (11 and 6-fold), and TFC (4 and 2-fold) for anise seed and hawthorn fruit extracts respectively. For the antioxidant activity, the process using X-20 showed an improvement of around 12-fold for anise extracts and 15-fold for hawthorn extracts for antioxidant activity. In terms of brix, the anise extracts saw a 3-fold increase and the hawthorn extracts saw a 4-fold boost after going through the X-20 membrane concentration process. Additionally, the X-20 membrane exhibits the highest retention rates for both anise and hawthorn extracts and is least affected by fouling during the concentration process.
Abstract
The food robotics revolution is driving a shift in the vending machine sector from conventional pre-packaged sales to on-site food manufacture. As these machines develop into small-scale food processing points, it is critical to guarantee food safety. The implementation of automated Clean-in-Place (CIP) techniques, in addition to manual cleaning, is modelled after food production practices, where hygiene is maintained without direct human intervention. These days, running these modern, multifunctional vending machines requires giving the highest priority to food safety and putting rigorous control measures in practice.
This case study aimed to implement a CIP procedure in a vending machine and assess microbial contamination. Water, blender, and smoothies were microbiologically analyzed to evaluate the microbial safety of ingredients, equipment, and the final product.
Microbiological analysis showed that none of the samples was contaminated with three major pathogens: Listeria monocytogenes, Salmonella spp., and Escherichia coli. This study showed the importance of the Clean-in-Place (CIP) process in automated vending machines.
Abstract
The aim of the present study was to find the best extraction parameters to obtain the highest amounts of polyphenols and antioxidants from the walnut. Walnut kernels from ‘Alsószentiváni 117’ cultivar were used for extraction. The extraction methods were as the follows:
Method 1: shaking water-bath at 50 °C for 30 min.
Method 2: shaking water-bath at 50 °C for 30 min, then storing at 5 °C for 20 h.
Method 3: shaking water-bath at 40 °C for 30 min.
Method 4: shaking water-bath at 40 °C for 30 min, then storing at 5 °C for 20 h.
According to our results Method 1 showed the highest FRAP value (34.43 mg AAE g−1), the DPPH value (52,94%) and the highest HPLC peaks for chlorogenic acid, epicatechin and rutin were also seen in extracts obtained using Method 1. TPC values of Method 3 were 26.06 mg GAE g−1 for Method 1 it was 25.65 mg GAE g−1. The results of color values, L* and ΔE* were similar in all extracts as well. In our experiments extraction Method 1 proved to be better than others.
Abstract
Ethylene has key roles in triggering and speeding up ripening processes, which in tomatoes take the form of various qualitative changes. Tomatoes, just like all climacteric fruits, need a continuous ethylene exposure to accelerate ripening. Therefore, it is possible to use ripening regulators preventing ethylene binding. According to some studies, chlorophyll fluorescence measurements can be used at least as efficiently as tristimulus colorimetry classifying tomatoes based on maturity. Measurements were carried out by treating fresh tomatoes with 1-MCP (1-methylcyclopropene) at six different stages of ripening and studying the changes in chlorophyll content related quality characteristics (e.g. surface colour, chlorophyll fluorescence) during postharvest storage (two-week refrigerated storage at 15 °C followed by a two-week shelf life). According to our results, chlorophyll content and photosynthetic activity of the treated samples decreased much less than those of untreated ones. Additionally, anti-ripening treatment proved to be more effective on tomatoes at an earlier stage of ripening.
Abstract
In this work, the simulated adulteration of coconut drink by dilution with water was investigated using laser-light backscattering (LLB) imaging. The laser vision system consisted of six low power laser modules, emitting 1 mm diameter beams at wavelengths of 532, 635, 780, 808, 850 and 1,064 nm. The backscattering images were acquired by a grey scale camera with 12 bit resolution. Eight parameters were extracted to describe the backscattering profile. The methods of linear discriminant analysis (LDA) and partial least squares (PLS) regression were performed on LLB parameters for classifying and predicting dilution level of adulterated coconut drink samples. Based on the results, LLB signals responded sensitively to adulteration. LDA results showed that adulterated samples were correctly recognized with accuracies between 60 and 100%. PLS models were able to estimate the adulteration level of samples with coefficients of determination of 0.57–0.97 in validation. This result demonstrated the potential of laser-light backscattering imaging as a rapid and non-destructive optical technique for evaluation of coconut drink adulteration.
Abstract
A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. Chromatographic separation was achieved with C18 (5 µm × 4.6 mm × 150 mm) column, at 30 °C with isocratic elution, mobile phase composed of solution A (acetonitrile), and solution B (0.5% formic acid) (65:35 v/v) at flow rate 1.2 mL min−1. The linearity range is 10–150 ng mL−1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. The retention time is 8.20 ± 0.02 min. LOD is found to be 3.3 ng mL−1 for drug. The method was applied to the analysis of SLP in human plasma with good recovery as 97.83%. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a prototype pharmacokinetic study by administration of 800 μg SLP to a healthy volunteer and parameters like AUC0–24, AUC0–∞, Cmax, tmax, and t1/2 were assessed.
Abstract
Atractylodis macrocephalae rhizome (AMR) belongs to medicine food homology. Its' clinical application of invigorating the spleen-stomach of AMR was applied to various diseases. In this research, a UPLC-QTOF-MS method was developed for qualitative and quantitative analysis of AMR, simultaneously. A Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm particle size) was used for separation of AMR multi-components. The column was eluted with a mobile phase of 0.1% formic acid-water and 0.1% formic acid-acetonitrile. Electron spray ionization with positive-ion mode and external standard method was utilized for quantifying the nine analytes in AMR. Constituents of AMR were scanned by UPLC-QTOF-MS and then identified by mass fragments and chromatographic information compared with the published literature and reference standards. Under positive mode, a total of 61 chemical compositions including 16 terpenoids, 8 polyacetylenes, 6 aromatics, 5 flavonoids, 5 coumarins, 5 organic acids, 4 amino acids, 3 fatty acids, 3 aliphatics, 2 steroids, and 2 alkenes, a nucleoside and an aldehyde were identified. Simultaneously, the contents of three amino acids (L-tyrosine, L-phenylalanine, and L-tryptophan), three sesquiterpenoids (atractylenolide Ⅲ, atractylenolide Ⅱ, and atractylenolide Ⅰ), a flavonoid (rutin), an organic acid (ferulic acid), and a pentacyclic triterpenoid (oleanolic acid) were determined in seventeen AMR batches. Amino acids and triterpenoid were quantified for the first time in AMR. The UPLC-QTOF-MS method developed in this article was reliable, practical, and useful for qualitative and quantitative evaluation of AMR multi-components.
Abstract
Coloring agents in foods and drinks have been popular for centuries. This study aims to analyze the presence of ten synthetic colors (namely, (allura red (E129), amaranth (E123), sunset yellow (E110), tetrazine (E102), fast green (E143), ponceau 4R (New Coccine) (E124), erythrosin B (E127), brilliant blue FCF (E133), brilliant black (E151) and carmoisine (E122))) in food and drink samples using ultra-high-performance liquid chromatography diode array detection (UHPLC-DAD). The present analytical method was carried out using Agilent Poroshell 120 HPH-C18 column, 3 × 100 mm, 2.7 µm, and a mobile phase consisting of 10 mM Na2HPO4, pH 7, mixed with methanol as a time-increment gradient solution until the time was 20 min, then decreased with time until the time was 26 min. The pH was set by orthophosphoric acid at 7 and 5 μL injection volume, 0.50 mL flow rate, and the elution systems were monitored at 428 nm for E102, 518 nm for E124, E110, E129, E122, 530 nm for E151, E127, 622 nm for E143, and E133, respectively. The limit of detection and quantification for all colors ranged from 0.017 to 0.025 and 0.057 and 0.082 mg L−1, respectively. The correlation coefficient values ranged between 0.9991 and 1.0. The selectivity of the assay revealed no interference from other components in the analyzed samples. The percent recovery and precision (intra- and inter-day) of the spiked samples were within the acceptable limits of the ICH guidelines. Five analytical parameters were employed, and the results showed a new, novel, and robust method according to ICH guidelines for analyzing these colors. While most of the investigated food and drinks fell within the accepted range, some fell outside. The current sample preparation and analytical methods are comprehensive and universal for extracting and measuring synthetic colors in various food and drink samples.
Talajnedvesség-tartalom mérése földradarral (GPR) és mezőgazdasági alkalmazhatóságának lehetőségei
Soil water content measurements with ground penetrating radar (GPR) and its application possibilities in the agriculture
Measurement of soil water content is complicated due to the soil heterogeneity and environmental variability. No single efficient method has been developed to map the different soil moisture zones at great depth at the field scale without disturbing the soil structure and paths of the waterflow.
Partially or completely non-destructive measurement of soil moisture is provided by ground-penetrating radar (GPR), which offers high resolution and significant penetration depth for medium-scale soil moisture measurements, bridging the methodological gap between small-scale point-based and large-scale remote sensing techniques. In addition, this technique can be used with better time efficiency compared to other destructive or non-destructive procedures.
GPR has been used for soil water content estimation including measuring soil water content profile, identifying specific soil water depths or soil water variation under irrigation conditions.
Despite the high potential of GPR for hydrological investigations, it is important to realize that no single geophysical method is able to perform optimally under all conditions. For example, GPR is mostly restricted to areas with relatively low electrical conductivity (low attenuation of the electromagnetic wave). In addition, some of the GPR interpretation methods require the presence of well identifiable and continuous GPR reflections, which requires sufficient and spatially continuous subsurface contrast in dielectric permittivity.
Soil moisture (considering its flow) is a key variable in the fields of agriculture. It is the essential requirement for plants to grow. Consequently, soil moisture is important for irrigation management particularly in semiarid and arid regions.
In this paper, the literature of the principles of GPR measurements and utilization possibilities is summarized with the emphasis on the agricultural sector. GPR can be a beneficial measuring device that can help in mapping soil moisture distribution, taking into account infiltration, but also water loss caused by evaporation and plant water absorption. Consequently, it can be used in agriculture, due to its precision at high central frequency values, even (fine)root characteristics of the plants, essentially the xylem-water relationship can also be determined (xylem transports water and water-soluble minerals and supply water used during photosynthesis). In addition, GPR can provide valuable information regarding natural stratification and soil compaction. The data interpretation of GPR measurements, in addition to soil compaction causing a decrease in the moisture of soils (as three-phase systems), can in principle be extended to other aspects of agrotechnology, such as soil contamination studying. However, it has not been sufficiently explored, as no recent literature can be found on this subject.
Soil radar can be a useful part of “Smart farming”, which can help in the selection of soil moisture measuring sensors placed in the soil as part of it. Especially when associated with the recently released new simultaneous multi-offset and multi-channel (SiMoc) GPR system, which enables fast soil profile mapping with seven receivers, but at the speed of a traditional single-channel GPR.
If complete non-destruction is the goal, air-coupled GPRs mounted on a drone can provide an opportunity. It should be noted, however, that due to the significant signal attenuation (wave scattering) occurring at the soil-air interface, only a small penetration depth can be achieved.
Abstract
In order to improve the thermal performance of heat exchangers and air collectors, we insert various forms of artificial roughness, known as ribs, into the useful duct. These ribs promote the creation of turbulent flows and enhance heat transfer by conduction, convection and radiation.
However, the introduction of these ribs leads to an increase in pressure drop, requiring higher mechanical power to pump the heat transfer fluid. This experimental study focuses on estimating, using empirical approaches, the pressure losses induced by rectangular ribs with an inclined top. The ribs are made from 0.4 mm galvanized sheet steel.
An experimental set-up was designed to measure the head losses generated by the ribs, from the point of entry to the point of exit from the useful duct. Using the dimensional analysis method, correlations were established to evaluate head losses as a function of flow regime and rib geometry and configuration (including different geometries for rib arrangement over the configuration area).
Abstract
An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of monocrotaline and usaramine in rat plasma, to study the plasma drug concentration and pharmacokinetics, and to calculate the absolute bioavailability. The plasma was treated with acetonitrile and methanol (9:1, v/v) protein precipitation method. The chromatographic column was UPLC HSS T3 (50 mm × 2.1 mm, 1.7 μm), the mobile phase was methanol-water (containing 0.1% formic acid with 10 mM ammonium acetate in water), and the elution time was 4 min at a flow rate of 0.4 mL min−1. Electrospray ionization (ESI) positive ion mode was used for detection and multiple reaction monitoring (MRM) mode was used for quantitative analysis. Monocrotaline and usaramine were administered sublingual intravenously (iv) 1 mg kg−1 and orally (po) 5 mg kg−1, respectively, with 6 rats in each group, for a total of 24 rats. Then the pharmacokinetic differences in rats were evaluated. For the UPLC-MS/MS method, the calibration curve showed good linearity in the range of 2–2,000 ng mL−1, where r was greater than 0.99. The precision, accuracy, recovery, matrix effect and stability results were all consistent with the requirements of biological sample detection methods. to provide scientific experimental basis for the basic research The bioavailability of monocrotaline and usaramine in rat plasma was calculated, which was 43.5 and 19.5%, respectively.
Abstract
Silica, as a stationary phase, has low separation efficiency accompanied by overlapping, broadened, and tailed peaks, so it needs to be modified to improve its efficiency. This study aims to develop a silica-based stationary phase modified by tetraethylene glycol (TEG) to separate phenolic compounds. Silica was modified by a chemical bond between silanol groups on the silica surface and TEG through a 3-glycidyloxypropylmethoxysilane reaction. The modified silica was packed into a capillary column and used to separate simple phenolic compounds consisting of phenol, pyrocatechol, and pyrogallol. A sample of 0.2 µL was injected into the capillary liquid chromatography and the mobile phase employed was acetonitrile 98% with a flow rate of 3 μL min−1. Elution was also done isocratically in this process and detection was carried out at a wavelength of 254 nm. The mixture of simple phenolic compounds was successfully separated in less than 7 min. The asymmetry factor and resolution were 1.43–2.12 and 1.72–5.43 respectively. The number of the theoretical plates ranged from 213 to 7,857. Columns containing Si-TEG stationary phase also separate phenolic compounds, which consist of gallic acid, syringic acid, ferulic acid, and caffeic acid. A sample of 0.2 µL was injected into the capillary liquid chromatography and successfully separated the mixture in less than 12 min. The samples were eluted isocratically using a mixture of methanol and 50 mM phosphate buffer pH 2.5 (8:92) with a flow rate of 3 μL min−1. The phenolic acids compounds were detected at a wavelength of 280 nm. The chromatogram showed four separate peaks. The asymmetry factor and resolution were 1.53–1.63 and 1.14–1.74, respectively, but the number of the theoretical plates was low, ranging from 190 to 796.
Abstract
Pinus merkusii Jungh & De Vries. has become increasingly gathered more attention from researchers because the plant has a range of folk medicinal uses. Heartwood plant is the major source of dehydroabietic acid (DHAA) and abietic acid (AA), which possesses several medicinal properties, such as antiviral, antimicrobial, antiobesity and anti-inflammatory. The research proposed herein a low-cost, fast, specific, uncomplicated, sensitive, precise reverse-phase high-performance liquid chromatography (RP-HPLC). This method was conducted and validated for evaluating an amount of DHAA and AA in ethanol extract and oral spray containing P. merkusii heartwood extract. Additionally, stability and antimicrobial activities against clinically isolated Streptococcus mutans of the oral spray were determined. The separation was achieved on Pursuit 200Å PFP column, 150 × 4.6 mm, particles of 3 µm with a flow rate of 1.0 mL min−1. Methanol and water (70:30 v/v) were used as eluent with an isocratic mode and sample analysis volume was set at 10 µL, at a detection wavelength of 210 and 245 nm. The developed HPLC method for analysis of DHAA and AA showed good linearity with correlation coefficients equal to 1. Moreover, other validation parameters, comprised of accuracy, precision, specificity and detection and quantitation limits of this method displayed excellent reliability, validity and sensitivity. This method could be an interesting alternative for quantitative measurement of P. merkusii heartwood extract, oral spray formulation and other P. merkusii heartwood extract preparations. The result from antibacterial tests suggested that the oral spray containing P. merkusii heartwood extract is able to inhibit the oral pathogens causing dental caries. The oral spray decreased S. mutans population size by about 0.5–2 Log CFU mL−1 at 1–4 h and complete elimination of all bacteria strains within 24 h. This study provides validity for using P. merkusii heartwood extract as an alternative for preventing and treating oral infectious diseases.
Abstract
In this study, we compile the findings to date on using several cellulose-based materials as adsorbents of potentially toxic elements (PTEs) from wastewater. Furthermore, this review discussed the destiny of PTEs-loaded cellulose-based adsorbents and some sustainable methods for their management, hoping to close the pollution loop.
Abstract
Mirtazapine is an antidepressant medication used to treat the major depressive disorder in adults. In this study, two different chromatographic methods were developed for the determination of mirtazapine in pharmaceutical products. In the first method, An Extend C18 column (250 × 4.6 mm, 5 μm) was used and the temperature was kept constant at 25 °C. The mobile phase was determined as 0.1% formic acid solution and acetonitrile (80/20, v/v), and isocratic elution was applied. The flow rate of the mobile phase was determined as 1.0 mL min−1 and the injection volume was 20 µL. Detection was performed at 291 nm. using a UV detector. In the second method, ethanol was used as the organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated by ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 µg mL−1. of mirtazapine. Later, these chromatographic methods were applied to pharmaceutical formulations. Comparison of the obtained results in terms of means was made using Student's (t) test, and comparisons in terms of standard deviations were made using the Fischer (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using the AGREE-Analytical GREEnness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of mirtazapine in pharmaceutical formulations.
Abstract
It still remains a great challenge to selectively enrich and sensitively quantify the trace volatile organic compounds (VOCs) in real samples with complex matrix. In this study, an integration method combining a selective enrichment medium of reduced graphene oxide (rGO) with a specially designed micro thermal-assisted purge-and-trap sampling device was developed for efficient enrichment and sensitive quantification of trace tobacco VOCs coupling with thermal desorption (TD)-gas chromatography/mass spectrometry (GC/MS). The prepared rGO has been proved to possess excellent enrichment selectivity and capacity for tobacco polar VOCs with the multi-layer structure, good thermal stability and large specific surface area. The specially designed sampling device was efficient and suitable for enriching and sampling trace polar tobacco VOCs coupling with rGO medium. Under the optimized sampling and analytical conditions, the established analytical method could be actually applied for quantification of typical tobacco polar VOCs with the good recoveries of 72.9–128% and the satisfied RSDs of 1.8–19.9% (n = 3). The results suggested that the developed method was selective, sensitive and reliable for enrichment and quantification of trace tobacco polar VOCs.
Abstract
A highly accurate and precise method for the simultaneous detection of 18 neonicotinoids and their metabolites in meat was developed using liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). To improve the pretreatment step of the method, five different commercially available clean-up materials (including C18+PSA (primary secondary amine), Z-Sep (with Discover DSC-C18), EMR-Lipid, SHIMSEN QuEChERS, and Clean-up LPAS) were studied in the treatment of three meat matrices: pork, duck and yellow croaker. Based on the recovery data, we found that among the five purification materials, SHIMSEN QuEChERS was slightly more effective than the others for 18 neonicotinoids. Therefore, SHIMSEN QuEChERS was used as the purification sorbent, and the extraction solvents, extraction methods and chromatographic and mass spectrometric conditions were optimized. A matrix-matched calibration method was applied for quantification. In three different meat matrixes (pork, duck, and yellow croaker), all the target compounds showed good linearity, both with values of r 2 > 0.995. The average recovery of all neonicotinoids ranges from 63.4 to 114.2% (pork), 63.0–113.2% (duck), and 63.9–110.5% (yellow croaker). Relative standard deviations were all <15% for intraday and interday precision. The values of limit of detection (LOD) and limit of quantification (LOQ) were, respectively, ranging from 0.04 to 1.0 μg kg−1 and 0.10 to 2.0 μg kg−1. Compared with previous reports, this method has advantage in LOQs, indicating that it it may be a preferred choice for the detection of neonicotinoid pesticides in meat samples.
Abstract
In our study, using a combination of eye-tracking parameter analysis and the van Westendorp method, we investigate whether participants pay more attention to products that they perceive as more expensive or to those that they prefer in the ranking process. The experiment involved 50 participants, a questionnaire with ranking and pricing tasks, and an eye-tracking measurement. Three wine varieties (Irsai Olivér, Rosé and Merlot-Shiraz) and three different label alternatives were tested. When comparing the results of the ranking and the pricing tasks, the product that is considered more expensive is not always the one that is most appealing to the participants. If we compare the results from the analysis of the eye-tracking parameters and the pricing, we can say that in all cases the labels that received the most visual attention were those that were priced more expensively by the participants.
Abstract
An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.
Abstract
A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank.
Abstract
The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R 2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument.
Abstract
Residues of the fungicides difenoconazole, propiconazole, cyflufenamid, and mandipropamid were determined in tomato fruit using acetonitrile for extraction and LC-MS/MS for quantification. Validation criteria include linearity range, the limit of detection (LOD) and limit of quantitation (LOQ), accuracy in terms of precision and trueness, and matrix effect were studied. The recovery rates of the method ranged from 91.8 to 106.3%. The precision of the method in terms of repeatability at one day (RSDr) and between three days (RSDR) ranged from 2.8 to 6.4% and from 4.3 to 7.6%, respectively, with good trueness from 92.2 to 96.4%. Matrix effects (suppression effects) ranged from 3.8% to 11.1%. The validated method was used to evaluate the dissipation kinetics of three different premix formulations: 30% EC (15% difenoconazole + 15% propiconazole), 14% DC (12.5% difenoconazole + 1.5% cyflufenamid), and 50% SC (25% difenoconazole + 25% mandipropamid) used on field tomatoes in Egypt. A first-order kinetic equation best describes residue dissipation. The calculated half-lives of difenoconazole, propiconazole, cyflufenamid, and mandipropamid were 2.01–2.27, 1.89, 1.97, and 1.71 days, respectively. The dissipation rate of difenoconazole did not differ significantly in the three premix formulations. Mandipropamid also dissipated faster compared to the other fungicides tested. The chronic dietary risk assessment results showed a minimal risk to adult Egyptian consumers. Waiting periods were advised for the safe consumption of tomatoes treated with the tested premix formulations.
Az azbesztszálak kimutatására szolgáló vizsgálatok középpontjában a levegőszennyezettségi értékek álltak, de a 21. században felmerült az igény a problémakör kiterjesztésére. Az elmúlt években megjelent nemzetközi tudományos szakirodalmak megcáfolták az évtizedeken át fennálló feltételezést, miszerint az azbeszt csupán a levegőterheltség révén vált ki kockázatot. Vízminőségi és talajminőségi kutatások által teret nyert az azbesztszálak, különösen a krizotilszálak alternatív transzportútjainak vizsgálatát célzó kutatásterület. Annak ellenére, hogy mind a települési, mind pedig a mezőgazdasági vízgazdálkodás potenciálisan érintett a krizotil-azbeszt jelenléte kapcsán, nincs nemzetközi szinten egységes és elfogadott módszer vagy küszöbérték az egyes vízforrások biztonságára vonatkozóan. A kutatások nyilvánvaló korlátja, hogy csekély mennyiségű és minőségű tudás érhető el. Az azbesztszálak megjelenése az egyes vízbázisokban jelentősen megváltoztatja mind a mezőgazdasági, mind a települési vízgazdálkodás környezeti hatásoknak való kitettségéről alkotott eddigi ismereteinket. Az öntözővizzel és a gyűjtött csapadékkal kijuttatott azbesztszálak hatásainak palettája mára túlhaladta a humán- és állategészségügyi hatásokat, immár figyelmet kell fordítani a vegetációs hatásokra is. Annak érdekében, hogy nagyobb betekintést nyerjünk az azbeszttoxicitás növényekre gyakorolt hatásaiba, sokkal több tudományos eredményre van szükség.
Jelen összefoglaló tanulmányban bemutatjuk az azbeszt, különös tekintettel a krizotil azbeszt legfontosabb tulajdonságait, humán-, állat- és növényegészségügyi kockázatait. Rávilágítunk arra, hogy ismereteink rendkívül hiányosak, valamint felhívjuk a figyelmet a települési és mezőgazdasági vízgazdálkodás érintettségének egyes faktoraira, közvetlen és közvetett kockázati tényezőire, valamint arra, hogy ezek miként hatnak az élőlényekre, kiemelt tekintettel a növényekre.
Abstract
A novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect.
Abstract
In this work, a UPLC-MS/MS assay was established for the determination of morphine, codeine, thebaine, papaverine and noscapine in rat plasma. ACQUITY UPLC BEH C18 column was employed for chromatographic separation with the mobile phase comprised acetonitrile-10 mmol L−1 ammonium acetate aqueous solution (0.05% aqueous ammonia) using gradient elution. Midazolam was used as internal standard (IS). Electrospray ionization (ESI) in positive-ion mode with reaction monitoring (MRM) was used for quantitative analysis. The calibration curves for morphine, codeine, thebaine, papaverine and noscapine demonstrated good linearity (r > 0.995) in the range of 5–500 ng mL−1 for morphine and codeine, and 1–100 ng mL−1 for thebaine, papaverine and noscapine. The intra-day and inter-day precisions of morphine, codeine, thebaine, papaverine and noscapine were within 15%, the intra-day and inter-day accuracies were 89–114%, the recovery was better than 65%, and the matrix effects were 96–112%. The developed UPLC-MS/MS assay was successfully applied in the pharmacokinetics of papaverine and noscapine.
Abstract
In this study, a UPLC-MS/MS method was developed for determination of pancratistatin in the mouse blood, and the pharmacokinetics of pancratistatin in mice after intravenous (5 mg kg−1) and intragastric (15 mg kg−1) administration was studied. HSS T3 column was used for separation with mobile phases of acetonitrile and 0.1% formic acid using gradient elution procedure. The blood sample was treated by protein precipitant with acetonitrile, midazolam was used as internal standard (IS). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, m/z 326.2→83.8 for pancratistatin and m/z 326.2→291.4 for IS in electrospray (ESI) positive interface. It showed a good linear in the range of 10–4,000 ng mL−1 (r > 0.998); the intra-day and inter-day precision was <15%, and the accuracy was 93%–105%. The recovery was better than 82%, and the matrix effect was 94%–105%. The developed UPLC-MS/MS method was fast, selective, and suitable for the pharmacokinetics of pancratistatin in mice.
Abstract
The rapid technological development that is still taking place today, with increasingly interconnected IT tools, is introducing dramatic changes. The development of computer programs is rapidly transforming traditional processes and the systems that support them. It is therefore natural that the fourth industrial revolution (Industry 4.0) and its impact on Hungarian companies is one of the key topics of our time. We conducted an exploratory quantitative survey, asking 140 managers of Hungarian small, medium and large enterprises about their current situation in the context of Industry 4.0. We sought to find out to what extent the specific R&D and innovation potential of Industry 4.0 is accepted, and whether it has already been introduced in the companies. On a qualitative side, 2 case studies and 3 interviews were conducted, in which structured interviews were used to further explore the issue. We aimed to find out where SMEs stood in terms of digital preparedness and what advantages, possible disadvantages, and goals they managed to identify. Our research showed that an increasing number of companies have already decided to take the first steps towards industrial digitalisation, which will completely transform their internal processes.
Abstract
A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250 mm × 4.6 mm, 5 µm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL·min−1 and a column temperature of 40 °C. The drift tube temperature of the evaporative light scattering detection system was set at 40 °C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r = 0.9993–0.9995) during the test ranges (119.1–1190.7 μg·mL−1 for 12-hydroxystearic acid, 10.7–107.4 μg·mL−1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg·mL−1, the limits of quantitation were 3.2 and 7.4 μg·mL−1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n = 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.
Abstract
Indapamide (Indp) and certain other diuretics have been abused in sports, therefore, having sensitive methods for its detection and assay in biological fluids (whole blood, plasma, serum, and urine) is of significant importance. The racemic mixture of Indp is being used as an active pharmaceutical ingredient among other commonly prescribed diuretics. The regulatory authorities and pharmaceutical industries demand analytical methods for successful enantioseparation of such molecules. The paper presents a critical overview of the scientific issues of the application of contemporary techniques involving various chromatographic approaches (with liquid or supercritical fluid as mobile phases) and capillary electrophoresis and method development, for drug screening, assay, bioequivalence studies and enantioseparation of indapamide with their results. It also covers the historical developments that led to significant breakthroughs in research and concise evaluations of research in the area.
Different types of chromatographic methods (HPLC, CEC, SFC etc) discussed herein provide an insight and a choice to select a method to (i) screen Indp for drug abuse, (ii) separate, isolate and quantify the enantiomers of Indp and (iii) investigate their pharmacokinetics as markedly different species and not as a total drug. The article evaluates the field's status with a broad base and practical oriented approach so that the underlying principles are easily understood to help chemists and non-specialists gain useful insights into the field outside their specialization and provide experts with summaries of key developments. To the best of authors' knowledge there has been no attempt to review such methods for analysis of Indp and this is the first report of its kind.
Rambutan (Nephelium lappaceum) production is growing worldwide so the treatment and utilization of Rambutan by-products has become a concern of manufacturers. The objective of this study was to evaluate the potential application of rhizobacteria to decompose Rambutan peel for organic fertilizer production. After the rhizospheric soil samples were selectively proliferated and preadded on agar medium containing only Rambutan peel, the rhizobacterial colony isolates were screened based on their ability to grow on this agar medium and then to degrade cellulose in Rambutan peel. The LD7.3 isolate from the Rambutan rhizosphere showed the highest efficiency in degrading Rambutan peel with 5.6% degraded cellulose content and was identified by the MALDI-TOF technique as belonging to Klebsiella. Klebsiella sp. LD7.3 grew well and maintained the same degrading activity after three times of subculturing in liquid medium. Notably, the supplementation of grinded Rambutan fruit peel to the liquid medium had a positive effect on the growth and the degrading activity of Klebsiella sp. LD7.3. This was the primary report on the application of rhizobacteria to degrade Rambutan peel and the results showed that this was a potential approach to reuse this waste source.
The experiment was conducted within a framework of a two-factor long-term trial at the Research Institute for Fisheries, Aquaculture and Irrigation, in Szarvas, Hungary. This was a special field experiment, in which lysimeters have been installed in the middle of 32 m2 field plots. The main factor was the water supply with 4 levels: i1: non-irrigated control; i2: irrigated with one third of the optimal water supply; i3: irrigated with two thirds of the optimal water supply; i4: optimum irrigated plot, according to the requirement of sweet corn test plant. The amount of released irrigation water was 0, 54, 106 and 158 mm per year on average over 5 years. Within every water supply treatment there were 4 nutrient supply rates (N): N1, N2, N3, N4 = 100, 200, 300 and 400 kg ha−1 NPK fertiliser substance in ratio 2:1:1. The number of replications was 4, and the experiment was arranged in split-plot design. In the studied years, the amount of precipitation varied between 92 and 264 mm from sowing to harvesting.
The effect of fertiliser was less in the non-irrigated treatments compared to that of the irrigated ones, and the yield was increased only up to 200 kg ha−1 NPK treatment level. The NPK dose of 300 kg ha−1 proved to be optimal in the irrigated treatments in which the utilization of fertilizer doses increased parallel to the improving water supply. In addition, the ratio of first class products (cobs longer than 20 cm) increased to a greater extent than the yield as a result of irrigation and fertilization. Water requirement of sweet corn proved to be between 400–450 mm resulting in an average yield of 20–24 t ha−1, of which 18–20 t ha−1 came from marketable cobs. The amount of evapotranspiration fluctuated between 270–440 mm during the five years, depending on the quantity of water supply, but it changed to a lesser extent than the amount of the yield. Increasing the fertilizer dose practically did not affect ET in non-irrigated plants, but increased it by 20–30 mm in irrigated ones. The change was not significant.
The productivity of ET was only 30–45 kg ha−1 mm−1 in the non-irrigated treatment, while it was 50–55 kg ha−1 mm−1 in the irrigated treatments, with higher values at the higher fertiliser rates. The productivity of irrigation water exceeded far over the productivity of ET at adequate nutrient supply. The yield increase per 1 mm of irrigation water was on average 60 kg ha−1 mm−1, which was considerably higher than the productivity of ET of non-irrigated plants (39 kg ha−1 mm−1). There was a positive correlation between the yield and ET, and a negative correlation between the yield and specific water consumption. Irrigation and fertilization increased the average yield to a greater extent than evapotranspiration, so as the average yield increased, the ET per unit of yield decreased, i.e. the productivity of evapotranspirated water increased.
Abstract
Pregabalin is a gabapentinoid approved for the treatment of general anxiety disorder, neuropathic pain and as adjunctive therapy for focal seizures in patients with epilepsy. In addition, there are a number of conditions for which pregabalin is prescribed off-label. Along with the widespread use there are a significant number of reports describing the misuse of pregabalin over the last decade. Over time, it became clear that pregabalin should become part of routine testing in toxicology laboratories. The aim of this paper was to present validation of a LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients. Simple sample preparation step and rapid chromatographic separation shortened the overall analysis time, which was the goal of method development. The presence of pregabalin was confirmed with three ion transitions, ensuring high selectivity of the validated method. The statistical data obtained showed good precision and accuracy over a wide concentration range. No endogenous or other interference was detected, and there was no matrix effect influence with this method. The LC-MS/MS method was applied to quantify pregabalin in plasma samples of patients admitted to the emergency department due to a possible acute pregabalin overdose. Different concentrations were found, and we report, to the best of our knowledge, the highest plasma concentration of pregabalin in the plasma of a patient with acute poisoning. In conclusion, we developed a fast and simple LC-MS/MS method for reliable determination of pregabalin and demonstrated the developed method was suitable for routine use in clinical toxicology setting.