Separations, Volume 9, Issue 7 (July 2022) – 29 articles

Superalloy scraps are deemed as potential unconventional sources of rare metals. In this study, an ultrasonic leaching method with a two-stage separation process was proposed. A series of Eh-pH diagrams for rare metals was constructed, and the results indicated that the leaching and separation process could be realized by adjusting the potential and pH values of leaching solutions. In the ultrasonic leaching process, results showed that the economic leaching percentages of Re, Ni, Co, Al, and Cr were 92.3%, 95.2%, 98.5%, 98.7%, and 97.5%, respectively. Compared with conventional leaching, ultrasonic leaching can improve the leaching percentages of rare metals by approximately 20%. In the two-stage separation process, the optimal recovery efficiencies of Al and Cr were 94.6% and 82.1% at a pH of 4.5, and Ni and Co were 99.5% and 98.3% at a pH of 7.5. With a two-stage precipitate process, rare metals can be efficiently recovered without generating any waste acid. Full article

A comparison between the classical gas chromatography (GC) technique with supercritical fluid chromatography (SFC) technology was performed using an essential oil of Citrus limon (lemon) as a model, considering its wide use in the cosmetic world. For the qualitative part, the signal annotation was achieved by mass spectrometry using either an electron ionization (EI) or an atmospheric pressure photoionization (APPI) source. For the quantitative part, GC was hyphenated to a flame ionization detector (GC-FID) and SFC to an ultraviolet detector (SFC-UV). The assay of the major component of citrus oil, i.e., limonene, was carried out by SFC-UV. The similar results obtained between GC-FID and SFC-UV allows SFC-UV to be considered as an alternative to GC-FID for Citrus oil characterization. Then, analyses of an essential oil collection from Citrus fruits were achieved to confirm the potential use of SFC-UV for oil classification in the context of quality control of raw materials in cosmetics. Full article

Three types of Zostera marina L. collection were extracted using the supercritical CO₂-extraction method. For the purposes of supercritical CO₂-extraction, old seagrass ejection on the surf edge, fresh seagrass ejection on the surf edge and seagrass collected in water were used. Several experimental conditions were investigated in the pressure range 50–350 bar, with the used volume of co-solvent ethanol in the amount of 1% in the liquid phase at a temperature in the range of 31–70 °C. The most effective extraction conditions are: pressure 250 Bar and temperature 60 °C for Z. marina collected in sea water. Z. marina contain various phenolic compounds and sulfated polyphenols with valuable biological activity. Tandem mass-spectrometry (HPLC-ESI–ion trap) was applied to detect target analytes. 77 different biologically active components have been identified in Z. marina supercritical CO₂-extracts. 38 polyphenols were identified for the first time in Z. marina. Full article

Amaranth (Amaranthus cruentus) is a possible alternative to high-nutritional-value crops. Amaranth seeds are considered to be one of the few sources of phytosqualene (up to 8%). The use of squalene and its hydrogenated form squalane in skincare formulations has been steadily increasing, and the demand for these compounds is expected to rise continuously. The aim of this study was to investigate the amaranth oilseed as a potential ingredient for cosmetic applications. First, an experimental design and optimization were carried out in order to obtain amaranth oil rich in squalane instead of squalene through catalytic hydrogenation. Under the optimal conditions, the resulting oil was fully hydrogenated, with higher stability, and more suitable for cosmetic uses. Furthermore, the effect of the addition of amaranth oil and squalane on the rheological and sensory characteristics of moisturizing cream formulations was assessed. As expected, higher contents of oil and polyunsaturated fatty acids were obtained by supercritical CO₂ extraction, and were used for the next step of the experiment. Optimization of the experimental conditions resulted in fully hydrogenated amaranth oil, with higher stability and rich in squalane. Better quality of moisturizing cream formulations was achieved when W/O formulations were enriched with 2% oil, or by adding 1% oil and 1% squalane. The formulation rich in squalane showed a better overall quality compared to other formulations. Full article

In order to recover lithium from brine with a high Mg²⁺/Li⁺ ratio, a positively charged nanofiltration (NF) membrane was prepared by depositing polydopamine (PDA)-coated graphitic carbon nitride (g-C₃N₄) as the interlayer (PDA-g-C₃N₄) and the interfacial polymerization (IP) of polyethyleneimine (PEI) and trimesoyl chloride (TMC) was carried out. Under optimal conditions, the water contact angle of the composite membrane is only 55.5° and the isoelectric point (IEP) is 6.01. The final positively charged NF membrane (M5) exhibits high permeance (10.19 L·m⁻²·h⁻¹·bar⁻¹) and high rejection of Mg²⁺ (98.20%) but low rejection of Li⁺ (13.33%). The separation factor (SF) is up to 48.08, and the Mg²⁺/Li⁺ ratio of the permeate is 0.036 in the simulated brine. In conclusion, the M5 membrane shows a good separation performance for salt lake brine (SF = 12.79 and Mg²⁺/Li⁺ ratio of the permeate = 1.43) and good fouling resistance. Therefore, the positively charged M5 membrane with PDA-g-C₃N₄ as the interlayer has the potential to be used for the recovery of lithium from brine. Full article

Cost-effective pretreatment of highly concentrated and bio-refractory petrochemical wastewater to improve biodegradability is of significant importance, but remains challenging. This study compared the pretreatment of petrochemical wastewater by two commonly used chemical advanced oxidation technologies (Fenton and ozone oxidation), and the mechanisms of biodegradability improvement of pretreated wastewater were explored. The obtained results showed that in the Fenton oxidation system, the COD removal of petrochemical wastewater was 89.8%, BOD₅ decreased from 303.66 mg/L to 155.49 mg/L, and BOD₅/COD (B/C) increased from 0.052 to 0.62 after 60 min under the condition of 120 mg/L Fe²⁺ and 500 mg/L H₂O_2, with a treatment cost of about 1.78 $/kg_COD. In the ozone oxidation system, the COD removal of petrochemical wastewater was 59.4%, BOD₅ increased from 127.86 mg/L to 409.28 mg/L, and B/C increased from 0.052 to 0.41 after 60 min at an ozone flow rate of 80 mL/min with a treatment cost of approximately 1.96 $/kg_COD. The petrochemical wastewater treated by both processes meets biodegradable standards. The GC–MS analysis suggested that some refractory pollutants could be effectively removed by ozone oxidation, but these pollutants could be effectively degraded by hydroxyl radicals (^•OH) produced by the Fenton reaction. In summary, compared with ozone oxidation, petrochemical wastewater pretreated with Fenton oxidation had high COD removal efficiency and biodegradability, and the treatment cost of Fenton oxidation was also lower than that of ozone oxidation. Full article

The single cell protein (SCP) technique has become a popular technology in recent days, which addresses two major issues: increasing world protein deficiency with increasing world population and the generation of substantial industrial wastes with an increased production rate. Global fruit production has increased over the decades. The non-edible parts of fruits are discarded as wastes into the environment, which may result in severe environmental issues. These fruit wastes are rich in fermentable sugars and other essential nutrients, which can be effectively utilized by microorganisms as an energy source to produce microbial protein. Taking this into consideration, this review explores the use of fruit wastes as a substrate for SCP production. Many studies reported that the wastes from various fruits such as orange, sweet orange, mango, banana, pomegranate, pineapple, grapes, watermelon, papaya, and many others are potential substrates for SCP production. These SCPs can be used as a protein supplement in human foods or animal feeds. This paper discusses various aspects in regard to the potential of fruit wastes as a substrate for SCP production. Full article

Boerhavia diffusa, also known as Punarnava, is a plant of the Nyctaginaceae family that has been utilized in traditional medicine to cure a variety of ailments. The goal of this study was to use response surface methodology (RSM) to optimize the maximum percentage yield of boeravinone B and caffeic acid from Boerhavia diffusa roots, and simultaneous determination of boeravinone B and caffeic acid in newly developed single solvent system and demonstrate the hepatoprotective benefits of boeravinone B and caffeic acid. The extraction process examined extraction time, extraction temperature and solvent concentration, which were optimized via Box–Behnken experimental design. The proposed HPTLC method for the quantification of boeravinone B and caffeic acid were successfully validated and developed. The method was validated in term of linearity and detection limit, quantification limit, range, precision, specificity and accuracy. The separation of boeravinone B and caffeic acid bands was achieved on HPTLC plate using formic acid: ethyl acetate: toluene (1:3:5 v/v) as developing system. Densitometric analyses of boeravinone B and caffeic acid was carried out in the absorbance mode at 254 nm. The maximum percentage yield of caffeic acid and boeravinone B from Boerhavia diffusa require appropriate extraction parameters such as temperature, time, organic solvents and water content, which can be achieved using the Box-Behnken statistical design provide time: temperature: solvent ratio (30:45:40 v/v) for extraction of caffeic acid and 60:60:40 v/v for extraction of boeravinone B. The boeravinone B (200 µg/mL) and caffeic acid (200 µg/mL) showed the most significant hepatoprotective activity compared with standard sylimarin in HepG2 cell induced with galactosamine 40 mM toxicity. The findings supported B. diffusa’s traditional use as a functional food forhuman health benefits. Full article

A reliable chromatographic strategy is crucial for the extraction of target compounds from natural sources as it is related to the preparation efficiency, as well as the purity of the compounds. In this study, medium-pressure normal-phase liquid chromatography and high-pressure reverse-phase liquid chromatography were combined to prepare and purify ergosterol from Tulasnellaceae sp. of Gymnadenia orchidis. First, Tulasnellaceae sp. was extracted three times (2.0 L and 2 h each time) with ethyl acetate, and the 6.0 L of extract solution was concentrated under reduced pressure to yield 2.2 g of crude sample. Then, the crude sample was pretreated utilizing silica gel medium-pressure liquid chromatography to enrich the target ingredient (586.0 mg). Finally, high-pressure reversed-phase liquid chromatography was used to purify the target compound, and the compound was characterized as ergosterol (purity > 95%) using spectral data. Overall, the simple and reproducible integrated chromatographic strategy developed in this study has the potential for the large-scale purification of steroids for laboratory and even industrial research. To the best of our knowledge, this is also the first report of ergosterol in Tulasnellaceae sp. Full article

Microsamples are collections usually less than 50 µL, although all devices that we have captured as part of this review do not fit within this definition (as some can perform collections of up to 600 µL); however, they are considered microsamples that can be self-administered. These microsamples have been introduced in pre-clinical, clinical, and research settings to overcome obstacles in sampling via traditional venepuncture. However, venepuncture remains the sampling gold standard for the metabolic phenotyping of blood. This presents several challenges in metabolic phenotyping workflows: accessibility for individuals in rural and remote areas (due to the need for trained personnel), the unamenable nature to frequent sampling protocols in longitudinal research (for its invasive nature), and sample collection difficulty in the young and elderly. Furthermore, venous sample stability may be compromised when the temperate conditions necessary for cold-chain transport are beyond control. Alternatively, research utilising microsamples extends phenotyping possibilities to inborn errors of metabolism, therapeutic drug monitoring, nutrition, as well as sport and anti-doping. Although the application of microsamples in metabolic phenotyping exists, it is still in its infancy, with whole blood being overwhelmingly the primary biofluid collected through the collection method of dried blood spots. Research into the metabolic phenotyping of microsamples is limited; however, with advances in commercially available microsampling devices, common barriers such as volumetric inaccuracies and the ‘haematocrit effect’ in dried blood spot microsampling can be overcome. In this review, we provide an overview of the common uses and workflows for microsampling in metabolic phenotyping research. We discuss the advancements in technologies, highlighting key considerations and remaining knowledge gaps for the employment of microsamples in metabolic phenotyping research. This review supports the translation of research from the ‘bench to the community’. Full article

Pulverized semi-coke was employed as raw material to prepare activated carbon via steam activation and evaluated as a CO₂ adsorbent. The effects of the preparation parameters including demineralization, activation temperature, activation time and steam flow on the structure and performance of the synthesized activated carbon were investigated. It was found that the microporous structure of activated carbon was greatly influenced by demineralization order and activation conditions. Demineralization before activation significantly increased the microporous structure of the activated carbon, which was ascribed to the removal of the inorganic fraction. Compared to the commercial activated carbon, activated carbon obtained by employing 150 mL/min steam to treat the demineralized pulverized semi-coke at 700 °C for 70 min possessed a higher CO₂/N₂ selectivity of 34.4 and good cyclic performance, which was due to its narrow microporosity of 0.55 nm. Furthermore, it was proved that a pore size of smaller than 1 nm is favorable for CO₂ sorption. Full article

The aim of this study was to investigate the correlation between solid materials and micropollutants, aiming to enhance the removal of the latter during the application of the ozonation process. For that purpose, two solid materials (SiO₂ and Al₂O₃) presenting catalytic activity were used for the removal of eight micropollutants from natural potable water, containing them either separately or in a mixture, by ozonation. The studied micropollutants, presenting different physicochemical properties, are atrazine, ibuprofen, p-CBA (ozone-resistant compounds), benzotriazole, caffeine (with moderate ozone reactivity), carbamazepine, fluoxetine, paracetamol (easily oxidized by ozone). The residual concentrations of carbamazepine, paracetamol, and fluoxetine were found to be lower than 5.9 μg/L, 1.2 μg/L, and 15.5 μg/L, respectively, after 1 min of oxidation time in all studied systems. In contrast, benzotriazole and caffeine removal was enhanced by the addition of catalysts; in both cases the best catalyst was SiO₂. Regarding the ozone-resistant compounds, both examined materials enhanced the removal of ibuprofen and p-CBA; however, the best was found to be SiO₂ and Al₂O₃, respectively. In contrast, Al₂O₃ cannot be considered as an effective catalyst for the removal of atrazine, which presents chemical affinity only with SiO₂ and for this reason it can be removed to a higher extent by its presence. Similar results were observed in the study of the mixture, although in this system, the residual concentration of all micropollutants was found to be under the detection limit after the application of catalytic ozonation. Full article

Azanza garckeana (F. Hoffm). Exell and Hillc. is an important food and medicinal plant that has been used in tropical Africa. Therefore, this study aimed to investigate the nutritional value of jakjak fruit using different analytical techniques. The obtained results have demonstrated that jakjak fruit is very rich in total soluble sugar, constituting about 48% of the dry weight. Moreover, the chromatographic analysis revealed that jakjak fruit contained a high amount of glucose, fructose, maltose, and ascorbic acid. Further, GC-MS analysis detected four compounds related to secondary metabolites. Some of these detected constituents have medicinal value. For example, phenol, 2,4-bis (1,1-dimethylethyl) has been reported to have many functions such as antioxidant activity, anticancer, antifungal, and antibacterial properties. Furthermore, the antioxidant potential of different concentrations of deionized water and methanolic extracts was estimated using 2,2-diphenyl-1-picrylhydrazyl (DPPH). The results showed that the scavenging activity of the DPPH radical was found to be raised with increasing concentrations of fruit extracts. The concentration (50%) of both methanol and deionized water gave the best inhibition percentage (91.7 and 84.4%), respectively. In contrast, the methanolic extract has shown significant results compared to deionized water. This study concluded that jakjak fruit is very rich in total soluble sugar and phenolic compounds, which can be used as a source of polysaccharides and antioxidants for the human diet as well as raw materials for downstream industries. Full article

Advanced treatment of biologically processed palm oil mill effluent (BIOTPOME), which possesses a potential danger to the water sources is required to meet the Malaysian discharge standard, as BIOTPOME contains high level of chemical oxygen demand (COD), suspended solids and oil and grease even after going through conventional treatment process. The significant but insufficient treatment efficiency of ponding system in Malaysia urged an alternative method to treat the recalcitrant organic compounds. Thus, post-treatment of BIOTPOME using oxidation by thermally activated persulfate process was proposed to solve this issue. In order to maximize the removal of COD and color, the central composite design (CCD) module of the response surface approach was used to optimize the interactions of the process variables temperature, S₂O₈²⁻/COD ratio, and reaction time. In order to identify the significant terms of interacting process factors, CCD performed a batch study from which statistical models of responses were created. All models were confirmed by analysis of variance (ANOVA) showing significances with Prob > F less than 0.1. The optimal performance was obtained at the temperature of 67.4 °C, S₂O₈²⁻/COD ratio of 9.8 and reaction time of 120 min, rendering COD removal of 85.65% and color removal of 85.74%. The total cost for the treatment process was RM0.94 per liter. Full article

Developing effective and green methods for food analysis and separation has become an urgent issue regarding the ever-increasing concern of food quality and safety. Ionic liquids (ILs) are a new chemical medium and soft functional material developed under the framework of green chemistry and possess many unique properties, such as low melting points, low-to-negligible vapor pressures, excellent solubility, structural designability and high thermal stability. Combining ILs with extraction techniques not only takes advantage of ILs but also overcomes the disadvantages of traditional extraction methods. This subject has attracted intensive research efforts recently. Here, we present a brief review of the current research status and latest developments regarding the application of IL-assisted microextraction, including dispersive liquid–liquid microextraction (DLLME) and solid-phase microextraction (SPME), in food analysis and separation. The practical applications of ILs in determining toxic and harmful substances in food specimens with quite different natures are summarized and discussed. The critical function of ILs and the advantages of IL-based microextraction techniques over conventional extraction techniques are discussed in detail. Additionally, the recovery of ILs using different approaches is also presented to comply with green analytical chemistry requirements. Full article

In this study, a needle–cylinder electrostatic precipitator with a water cooling system was designed to enhance the harvest of atmospheric water in wet flue gas. The effects of flow rate, temperature and particles on the collection of fog droplets were investigated. Meanwhile, the energy efficiency of water collection was analyzed at different voltages. The results show that the current decreases with the increase of air relative humidity under the same voltage, and the breakdown voltage increases obviously. Concurrently, by appropriately reducing the wet flue gas flow velocity, the residence time of fog droplets in the electric field can be increased, fully charging the droplets and improving the water collection efficiency. Moreover, experiments revealed that through decreasing the flue gas temperature, both the water collection rate and energy efficiency can be improved. In addition, the presence of particles in wet gas can improve the water collection rate by 5~8% at different discharge voltages. Finally, based on energy efficiency analysis, with the increase of voltage, although the water collection rate increased, the energy efficiency decreased. Full article

The deposited particulate material within a fibrous filter affects the pressure drop which develops through three different stages. The implementation of a time-adjustable matrix is intended to cause detachment of particle structures from fibers within the upstream layers at low flow velocities. The deposited particle structures are transported further within the filter and clear up void space for an extension of filter service life. As in previous studies observed fiber stretching initiate cracks and following detachment of particle structures with a simultaneously applied airflow. For complete detachment of the particle structure, five consecutive stretching cycles are performed in this study. The elongation velocity, the flow velocity and the particle loading are varied. Using an image analysis technique and a laser-light measurement technique simultaneously, the cumulative fraction of detached particle structures and the size of detached particle structures are determined. A high initial particle loading on the fiber induces early detachment of larger structures from the fiber. The size of detached structures is increased by the increase of the elongation velocity. The mean value remains almost constant whether the elongation velocity or superficial velocity are increased. For small initial structures on the fiber, a decrease in superficial velocity causes detachment of larger particle fragments. Full article

Cydonia oblonga miller (quince) plant serves as a potential folk medicine for treating hypertension and cardiovascular diseases in China. However, to the best of our knowledge, no study has been conducted on the polyphenolic profile and anti-adipogenic effect of quince fruit grown in China. In the current study, we aimed to investigate the quince fruit extract’s major phenolic compounds, evaluate their antioxidant activity, and examine their effect on adipogenesis in 3T3-L1 cells. A rapid and sensitive analytical method was established for the simultaneous determination of major polyphenolic compounds by using ultra-pressure liquid chromatography coupled with a triple quadrupole mass spectrometer (UPLC-MS/MS). Among the 10 compounds, the cryptochlorgenic acid was noticed as the most abundant compound of both purified (242.44 ± 0.73 µg/mg dw) and unpurified extract (3.37 ± 0.01 µg/mg dw) followed by quercetin 3-rutinoside and chlorogenic acid. Alternatively, both extracts possessed a high quantity of phenolic acids (purified extract = 483.10 ± 5.16 µg/mg dw and unpurified extract = 7.89 ± 0.02 µg/mg dw). The purified extract exhibited a strong antioxidant capacity (DPPH: EC50 = 3.316 µg/mL, ABTS: EC50 = 36.38 µg/mL) as compared to the unpurified extract. Additionally, our results also showed that the extract at 100 µg/mL significantly suppressed the preadipocyte differentiation and decreased the lipid droplets up to 69% in mature adipocytes. The present study highlights an accurate and fast detection method for quince fruit extract polyphenolic compounds with its antioxidant and antiadipogenic effects. The study also provides the necessary information for the rational development and utilization of quince fruit extract as a source of phytochemicals. Full article

Water pollution, resulting from the degradation of plastics into microplastics, exposes humans and other living organisms to contaminated drinking water. Microplastics are capable of adsorbing toxic heavy metals which are carcinogenic and may affect the reproductive functions of living organisms. Hence, this study focuses on the characterization and quantification of microplastics in water to raise the awareness and propose a method of dealing with this emerging pollutant in various aqueous environments. The microplastics were separated from water using polyvinylidene difluoride (PVDF) and PVDF modified with carbon nano-onions (CNOs). The PVDF exhibited the highest concentration of microplastics in the wastewater influent (140 ± 1.85 MP/L) compared to the effluent (8.8 ± 2.10 MP/L), tap water (6.5 ± 5.77 MP/L), and lake water (10 ± 2.65 MP/L). The stereo microscope displayed red, blue, and black colored plastics. The morphological properties were determined using SEM. ATR-FTIR, equipped with Spectrum 10 Spectroscopy Software was used to establish the presence of high-density polyethylene (50%), poly(1,4-butylene terephthalate) (16.6%), nylon 12 (16.6%), and cellulose (16.6%) in the influent. The quantification of heavy metals extracted from the microplastics indicated that the concentrations of As (1.759 to 8.699 mg/L), Cu (83.176 mg/L) and Zn (0.610 mg/L) were above the acceptable limits. Our work is beneficial for the development of a microplastics monitoring protocol for various municipalities. Water treatment plants may also include the treatment of microplastics in the influent and monitor the effluent before the water is released back into the environment. Full article

Polyphenols are natural antioxidants and play a vital role in inhibiting oxidative stress induced by the body’s free radicals. Banana peels are a significant agro-industrial waste. This waste could be utilized to extract polyphenols to process various functional foods and nutraceuticals. An investigation was executed to extract polyphenols from banana peel using the sonication and maceration techniques. Three different polar solvents, methanol, ethanol and acetone, were used at four different concentrations: 25%, 50%, 75% and 100%. Yield (%), Total Polyphenolic Content (TPC), Total Flavonoid Content (TFC) and 1,1-diphenyl-2-picryl-hydrazyl (DPPH) Radical Scavenging assays were performed. The results from the current study articulate that extraction by sonication yields a higher quantity of polyphenols than the maceration technique. The study also concludes that ethanol leads to better extraction than other solvents used in this study. Full article

Protein purification is a complex and non-standardized process; the fact that proteins have different structural types making it difficult to create a standard methodology to obtain them in a pure, soluble, and homogeneous form. The present study shows the selective development of a buffer suitable for proteins of interest that allows high concentrations of hGPN2 protein to be obtained with low polydispersion and high homogeneity and purity. By taking the different reagents used in the construction of different buffers as a basis and performing purifications using different additives in different concentrations to determine the optimal amounts, the developed process helps to minimize the bonds, maintain solubility, release the proteins present in inclusion bodies, and provide an adequate environment for obtaining high concentrations of pure protein. GPN proteins are of unknown function, have not been purified in high concentrations, and have been found as part of the RNA polymerase assembly; if they are not expressed, the cell dies, and overexpression of certain GPN proteins has been linked to decreased survival in patients with invasive ductal carcinoma breast cancer types ER+ and HER2+. The results of the present study show that the use of the buffer developed for recombinant hGPN2 protein expressed in Escherichia coli could be manipulated in order to isolate the protein in a totally pure form and without the use of protease inhibitor tablets. The resulting homogeneity and low polydispersion was corroborated by studies carried out using dynamic dispersion analysis. Thanks to these properties, it can be used for crystallography or structural genomics studies. Full article

To better control the quality of saponins, ensure their biological activity and clinical therapeutic effect, and expand the development and application of saponins, this paper systematically and comprehensively reviews the separation and analytical methods of saponins in the past decade. Since 2010, the electronic databases of PubMed, Google Scholar, ISI Web of Science, Science Direct, Wiley, Springer, CNKI (National Knowledge Infrastructure, CNKI), Wanfang Med online, and other databases have been searched systematically. As a result, it is found that ionic liquids and high-performance countercurrent chromatography are the most popular extraction and separation techniques for saponins, and the combined chromatography technique is the most widely used method for the analysis of saponins. Liquid chromatography can be used in combination with different detectors to achieve qualitative or quantitative analysis and quality control of saponin compounds in medicinal materials and their preparations. This paper provides the latest valuable insights and references for the analytical methods and continued development and application of saponins. Full article

The essential oils and polysaccharides from guava leaves have important functions. In the process of microwave extraction of plant essential oils and polysaccharides, pretreatment with lithium salts solution is helpful to increase the extraction rate. The experiment was conducted using a single factor method. Results were optimized by principal component analysis and response surface optimization. The optimal conditions were: LiCl dosage 45 μmol, microwave time 40 min, liquid-solid ratio 10, homogenization time 4.2 min, liquid-material ratio 10, and microwave irradiation power 700 W. The highest yield of essential oil and polysaccharide were 10.27 ± 0.58 mL/kg dry weight (DW) and 50.31 ± 1.88 g/kg·DW, respectively. Three verification experiments showed that the extraction rate of the microwave method was higher than that of the traditional heating method. In addition, the bacteriostatic zones reached the maximum 23.7 ± 0.11 mm when the concentration was 40 μL/mL, and the above results have practical significance. Full article

To verify the anti-fungus properties of the crop-harmful pseudocercospora, the essential oil (EO) of pomelo peel (PP) was extracted by a single factor combined with response surface optimization. Meanwhile, the composition and activity of EO were studied. The PP was squeezed by a screw extruder and pretreatmented by pectinase, then extracted by microwave-assisted steam distillation. The optimal conditions were as follows: pectinase dosage was 69.17 μmol/g, microwave power was 651.42 W and extraction time was 43.84 min. The dry weight (DW) yield of PPEO reached 14.63 mL/kg DW after BBD optimization. There were 23 compounds in the PPEO identified by GC-MS. Limonene, α-phrenbutene, and laurene in PPEO accounted for 79.31%, 4.72%, and 3.46%, respectively. In addition, the antifungal was effective when the concentration of PPEO was 3.5 mg/mL. Therefore, this study has guiding significance for the development of natural resources. Full article

Two-phase flow is very important in many areas of science, engineering, and industry. Two-phase flow comprising gas and liquid phases is a common occurrence in oil and gas related industries. This study considers three flow regimes, including homogeneous, annular, and stratified regimes ranging from 5–90% of void fractions simulated via the Mont Carlo N-Particle (MCNP) Code. In the proposed model, two NaI detectors were used for recording the emitted photons of a cesium 137 source that pass through the pipe. Following that, fast Fourier transform (FFT), which aims to transfer recorded signals to frequency domain, was adopted. By analyzing signals in the frequency domain, it is possible to extract some hidden features that are not visible in the time domain analysis. Four distinctive features of registered signals, including average value, the amplitude of dominant frequency, standard deviation (STD), and skewness were extracted. These features were compared to each other to determine the best feature that can offer the best separation. Furthermore, artificial neural network (ANN) was utilized to increase the efficiency of two-phase flowmeters. Additionally, two multi-layer perceptron (MLP) neural networks were adopted for classifying the considered regimes and estimating the volumetric percentages. Applying the proposed model, the outlined flow regimes were accurately classified, resulting in volumetric percentages with a low root mean square error (RMSE) of 1.1%. Full article

Aspalathus linearis (Burm.f.) R. Dahlgren, commonly known as rooibos tea, was consumed traditionally by the indigenous South African inhabitants as an herbal remedy. Beside antioxidant properties, it displays antiallergic, antispasmodic, and hypoglycemic activities. An ultra-high-performance liquid chromatography method coupled with photodiode array and mass spectrometry detectors were developed for the determination of 14 phenolic constituents from leaves and stems of A. linearis. The efficient separation was performed within 30 min at a temperature of 30 °C by using C-18 column as the stationary phase and water/acetonitrile with 0.05% formic acid as the mobile phase. Method validation for linearity, repeatability, limits of detection, and limits of quantification was achieved. The limits of detection from 0.2–1 μg/mL were reported for the standard compounds. Their total content varied substantially (1.50–9.85 mg/100 mg sample) in 21 dietary supplements. The presence of regioisomers and diastereomers which co-elute on a variety of stationary phases make separation for quantification purposes challenging. This method was found to be efficient in providing low retention times and excellent resolution for this type of phytochemicals. The established method is suitable for chemical fingerprint analysis of A. linearis and cost-effective for quality control of rooibos tea products. Full article

This article describes the validation of analytical methods for the determination of Manganese (Mn) and lead (Pb) by graphite furnace atomic absorption spectrometry (GFAAS) in human hair and nail samples. Method validation parameters such as linearity, repeatability, reproducibility, and precision were determined. In addition, the limit of detection (LOD), the limit of quantification (LOQ), and measurement uncertainty were calculated. The developed method was linear in the concentration ranges of 0.001–0.015 and 0.002–0.020 µg·L⁻¹ of Mn and Pb, respectively. The determination coefficients obtained were greater than 0.995. The recoveries obtained after the addition of the standard concentration for the metals ranged from 84.80–107.98%, with a precision not exceeding 12.97% relative standard deviation. The calculated LOD and LOQ for Mn and Pb are within the ranges established by Commission Regulation (EU) No. 836/2011. The expanded uncertainty was estimated to be less than 9.93–6.59% for Mn and Pb. Matrix effects were also studied, finding a smooth effect in both matrices. The analysis of 30 samples of each type revealed the presence of Mn in 30 and Pb in 13 samples. Overall, the proposed validation method was considered optimal for the determination of Mn and Pb. Full article

The enantioseparation of syn- and anti-3,5-disubstituted hydantoins 5a–i was investigated on three immobilized polysaccharide-based columns (CHIRAL ART Amylose-SA, CHIRAL ART Cellulose-SB, CHIRAL ART Cellulose-SC) by high performance liquid chromatography (HPLC) using n-hexane/2-PrOH (90/10, v/v) or 100% dimethyl carbonate (DMC) as mobile phases, respectively, and by supercritical fluid chromatography (SFC) using CO₂/alcohol (MeOH, EtOH, 2-PrOH; 80/20, v/v) as a mobile phase. The chromatographic parameters, such as separation and resolution factors, have indicated that Amylose-SA is more suitable for enantioseparation of the most analyzed syn- and anti-3,5-disubstituted hydantoins than Celullose-SB and Cellulose-SC in both HPLC and SFC modalities. All three tested columns showed better enantiorecognition ability toward anti-hydantoins compared to syn-hydantoins, both in HPLC and SFC modes. We have demonstrated that environmentally friendly solvent DMC can be efficiently used as the mobile phase in HPLC mode for enantioseparation of hydantoins on the immobilized polysaccharide-based chiral stationary phases. Full article

Numerous agents with anxiolytic or stimulant effects have the potential to be overused, and their misuse is associated with serious side effects. In Saudi Arabia, the estimated percentage of Saudis who abuse drugs is around 7–8% and the age range is 12–22 years. Methamphetamine, captagon, tramadol, heroin, and cannabis/cannabinoids have been proven to be the most commonly abused drugs in Saudi Arabia, with methamphetamine being at the top of the list. The present study focuses on the chromatographic analytical methods used for the analysis of methamphetamine in combination with commonly abused drugs, aiming to point out the greenest among them. These mixtures have been chosen as they are analyzed periodically and frequently in criminal evidence and forensic medicine. Therefore, the chances of hazards for analysts and the environment are high if the mixtures are not handled appropriately. This study aims to compare 23 chromatographic methods used for the analysis of methamphetamine mixtures in four major combinations, and to assess their greenness by using three greenness assessment tools, namely, NEMI, ESA and AGREE, to recommend the greenest analytical method. The NEMI results were proven to have low discriminating abilities and, accordingly, the comparisons are based on ESA and AGREE scores. The analysis results show that the safest methods with the most eco-friendly results (based on ESA and AGREE) are the GC-MS method proposed by Mohammed et al. to analyze methamphetamine and captagon mixtures (ESA = 79 and AGREE = 0.57), the UHPLC–MS-MS method proposed by Busardò et al. to analyze methamphetamine and cannabis/cannabinoid mixtures (ESA = 78 and AGREE = 0.57), the LC-MS method proposed by Herrin et al. to analyze methamphetamine and tramadol mixtures (ESA = 81 and AGREE = 0.56), and the LC-MS method proposed by Postigo-et al to analyze methamphetamine and heroin mixtures (ESA = 76 and AGREE = 0.58). Full article