Ethyl Acetate Solution Research Articles

Novel Organic Solvent Nanofiltration Approaches for Microbial Biosurfactants Downstream Processing.

Glycolipid biosurfactants are the most prominent group of microbial biosurfactants, comprising rhamnolipids, sophorolipids and mannosylerythritol lipids (MELs). Usually, large amounts of hydrophobic substrates (e.g., vegetable oils) are used to achieve high titers (~200 g/L) of a crude product of low purity at values limited to 50-60%, contaminated with unconsumed triacylglycerol and residual free fatty acids and monoacylglycerides. The methods reported for the removal of these contaminants use a mixture of organic solvents, compromising solvent recyclability and increasing final process costs. This study reports, for the first time, an innovative downstream method for MELs, in which 90% of the triacylglycerols are separated from the crude MEL mixture in a first stage and the other lipid derivatives (free fatty acids, mono- and diacylglycerols) are removed by organic solvent nanofiltration (OSN). Three commercially available membranes (GMT-oNF-2, PuraMEm-600 and DuramMem-500) and several homemade membranes, casted from 22, 24 or 26% (w/v) polybenzimidazole (PBI) solutions, were assessed for crude MELs purification by diafiltration. A final purity of 87-90% in the MELs was obtained by filtering two diavolumes of methanol or ethyl acetate solutions through a PBI 26% membrane, resulting in MELs losses of 14.7 ± 6.1% and 15.3 ± 2.2%, respectively. Higher biosurfactant purities can be archived using the PBI 26% membrane at higher DV, but at the cost of higher product losses. Namely, in MeOH, the use of 6 DV leads to losses of 32% for MELs and 18% for sophorolipids. To obtain MELs at reagent grade with purities equal or higher than 97%, a two-sequential cascade filtration approach was implemented using the commercial membrane, GMT-oNF. In such a process, MELs with 98% purity was obtained at the cost of 11.6% MELs losses. Finally, decoloration, important in some applications, was successfully assessed using activated carbon. Overall, this study reports a unique solution for microbial biosurfactants production with minimal product losses, enabling solvent recycling and potentially reducing costs.

Crystal structure and properties of anhydrous 5-nitroaminotetrazole

5-Nitraminotetrazole (5-NAT) is a high-energy and green explosive material that has attracted extensive attention due to its short synthesis steps and decomposition products consisting mainly of nitrogen and water. However, the presence of a crystal water molecule in the current crystal structure of 5-nitroaminotetrazole significantly affects its detonation performance and mechanical sensitivity. In this study, we report the successful synthesis of an anhydrous crystal form of 5-NAT through slow volatilization of an ethyl acetate solution under dry conditions. The anhydrous crystal form of 5-NAT exhibited increased density and detonation velocity compared to the monohydrate crystal form. Furthermore, quantum chemical analysis showed that the anhydrous crystal form exhibited increased sensitivity to external force stimulation due to stronger oxygen-oxygen and nitrogen-oxygen repulsion. In conclusion, the anhydrous crystal form of 5-NAT shows promise as a high-energy and green primary explosive.

General Approach to Silica-Supported Salens and Salophens and Their Use as Catalysts for the Synthesis of Cyclic Carbonates from Epoxides and Carbon Dioxide.

General routes for the synthesis of silica-immobilized symmetrical and unsymmetrical salophen and salen ligands and metal complexes have been developed starting from the natural product 4-allylanisole (methyl-chavicol and estragole). The key step of the syntheses is a microwave-assisted, platinum oxide catalyzed hydrosilylation of the terminal alkene of 5-allyl-2-hydroxybenzaldehyde to afford a sol-gel precursor which can be immobilized into silica before or after conversion to salen and salophen ligands to afford unsymmetrical and symmetrical silica-supported ligands, respectively. Both the symmetrical and unsymmetrical silica-supported salophens were found to catalyze the formation of cyclic carbonates from epoxides and carbon dioxide with catalytic activities at least comparable to those previously reported for non-immobilized homogeneous salophens. This reaction could also be carried out in a multi-phase flow reactor using ethyl acetate solutions of 3-phenoxypropylene oxide. Metal complexes of the silica-immobilized ligands could be prepared, and the aluminum complexes were also found to catalyze cyclic carbonate formation.

Comparison of solvents for extraction of Pachira macrocarpa (Cham. et Schlecht.) Walp seed oils

This study compared the lipid yield, chemical composition, thermal and rheological behavior of Pachira macrocarpa seed oil (PSO) extracted with five different solvents (petroleum ether, n-hexane, ethyl acetate, isopropanol and Folch solution (methanol/chloroform, v/v = 1: 2)). The results showed that the lipid yield of PSO extracted with ethyl acetate was the highest (29.25%). The main fatty acids of PSOs extracted by different solvents were palmitic acid (48.82–49.24%), linoleic acid (31.23–31.62%) and oleic acid (13.88–14.26%). Ethyl acetate was the most suitable solvent for extracting phytosterols (1756.43 mg/kg), n-hexane was the best solvent for enriching squalene (906.50 mg/kg), and isopropanol extraction was the most suitable for enriching tocopherols (436.90 mg/kg). Folch solution extraction can efficiently extract polyphenols and its oil had the best oxidative stability in all samples. Furthermore, PSOs showed high thermal stability and exhibited Newtonian flow behavior. Overall, this study provides guidance for the industrial production of PSO, and Folch solution extraction was the most suitable method for the development of PSO for the potential healthcare application.

Immobilization of Metronidazole on Mesoporous Silica Materials

Metronidazole (MTZ) is a widely used drug, but due to its many side effects, there is a growing trend today to use a minimum dose while maintaining high efficacy. One way to meet this demand is to reduce the size of the drug particles. A relatively new method of size reduction is attaching the drug molecules to a mesoporous carrier. In this paper, we studied the fixation of MTZ molecules on mesoporous silica carriers. The drug was immobilized on two mesoporous silica materials (Syloid, SBA-15) with the use of a variety of immersion techniques and solvents. The immobilized drug was subjected to physicochemical examinations (e.g., SEM, XPS, XRD, nitrogen uptake, DSC) and dissolution studies. A significantly higher immobilization was attained on SBA-15 than on a Syloid carrier. Among the processing parameters, the type of MTZ solvent had the highest influence on immobilization. Ultrasonic agitation had a lower but still significant impact, while the concentration of MTZ in the solution made no difference. Under optimal conditions, with the application of an ethyl acetate solution, the surface coverage on SBA-15 reached as much as 91%. The immobilized MTZ exhibited a ca. 10% faster dissolution rate as compared to the pure micron-sized drug particles.

Bioassay-Guided Characterization, Antioxidant, Anti-Melanogenic and Anti-Photoaging Activities of Pueraria thunbergiana L. Leaf Extracts in Human Epidermal Keratinocytes (HaCaT) Cells

Although the roots and flowers of P. thunbergiana are known to have various physiologically active effects, studies on the anti-melanin production and anti-photoaging effects of its leaf extracts and cellular mechanisms are still lacking. In this study, we evaluated the possibility of using Pueraria thunbergiana leaves as a natural material for skin whitening and anti-aging-related functional cosmetics. The 30% ethyl alcohol (EtOH) extract from P. thunbergiana leaves was fractionated using n-hexane, ethyl acetate (EtOAc), butanol, and aqueous solution to measure their whitening, and anti-aging effects. The EtOAc fraction contained a high content of phenolic and flavonoids and showed higher 1,1-diphenyl-2-picryhydrazyl (DPPH) and 2,2-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS) radical scavenging activities than the other fractions. It was also confirmed that the EtOAc fraction markedly inhibited α-melanocyte stimulating hormone (α-MSH)-induced melanogenesis in B16F10 melanoma cells. In addition, the EtOAc fraction showed a protective effect against ultraviolet B (UVB) in HaCaT cells and increased the collagen synthesis that was decreased due to UVB exposure. Matrix metalloproteinase-1 (MMP-1) activity and MMP-1 protein expression were reduced in human epidermal keratinocytes (HaCaT) cells. These results indicate that the EtOAc fraction has superior antioxidant activity, anti-melanogenesis, and anti-photoaging effects compared to the other fractions. Therefore, in this study, we confirmed the potential of P. thunbergiana leaf extract as a functional cosmetic ingredient, and it can be used as basic data for the physiological activity of P. thunbergiana leaf extracts.

MODIFICATION OF CERAMIC MEMBRANES BY PYROCARBON FROM CARBONIZED POLY(URETHANE UREA)S

Modification of tubular ceramic membranes made of clay minerals, which were obtained by slip casting (produced by the Dumansky Institute of Colloid Chemistry and Water Chemistry of the National Academy of Sciences of Ukraine) was carried out. The membranes were modified with pyrocarbon, which was obtained by carbonization of a precursor – poly(urethane urea)s. The carbonization precursor was synthesized from polyisocyanate (average functionality 2.7) and laprol grade 5003, which was introduced into the membrane by impregnation of the corresponding solutions in ethylacetate. When laprol reacts with polyisocyanate, three-dimensional polyurethane is formed. Since undried reagents were used, water entered the pores of the membrane, which reacted with the NCO groups of the polyisocyanate to form polyurea. The parallel course of these reactions leads to the formation of poly(urethane urea)s in the pores of the membrane. Carbonization was carried at 800 °C in an argon flow. The apparent density and open porosity of the membranes were determined by CCl4 uptake. After modification, the open porosity of the membrane decreased from 29.9 to 27.3 %, the apparent density increased from 1.86 to 1.87 g/cm3. The composition and structure of the membranes were studied by X-ray diffraction analysis and SEM. It is shown that the obtained modifier is pyrocarbon - the relative intensity of reflexes increases at 26,0 - 26,4 and 41,3 and 44,2° 2Θ. Pyrocarbon covers the surface of the pores with a continuous layer, and there are also three-dimensional formations of various shapes and sizes from several nm to several microns. Testing of modified membranes was carried out by water purification from direct scarlet dye and from Ca2+ of calcium chloride using the baromembrane method at a working pressure of 0.7 MPa. The unmodified membrane does not retain direct scarlet dye and Ca2+ at all. Tests of modified membranes have shown that the membranes acquire ultrafiltration properties. The retention factor (R) for direct scarlet dye is 100 % and 25 % for Ca2+.

Invitro Activity and Docking Approach In Silico Leaf Extract Syzygium polyanthum (Wight) Walp. as a Salmonella typhi Inhibitor

Indonesian people had long used plants as traditional medicine. In addition to maintaining health, traditional medicine was in great demand and prevents disease. We often encounter syzygium polyanthum leaves as a complement in tamarind and pepes, which were believed to act as a preservative. This study aimed to determine qualitatively bay leaf extract as an antimicrobial, Salmonella typhi. Methanol extraction of syzygium polyantum leaves would be partitioned with hexane and ethyl acetate solvents. The anti-microbial potential was shown in the Maximum Inhibitory Concentration (MIC) test, the identification of the compound using GC-MS and its potential as antibacterial was shown by docking the molecule using docking in silico technique against 5L3J protein. The MIC results were shown that the hexane partition at 100 ppm had 22.09 mm inhibition and the ethyl acetate partition at 80 ppm, had 18.15 mm inhibition. The GC-MS’ testing resulted of syzygium polianthum leaf extract showed the presence of alpha-pinene, alpha-cubenene, 1H-Cyclopropa [a] naphthalene, nerolidol, humulene epoxide II, phytol, 9,12,15-Octadecatrien-1-ol, Squalene, Alpha-tocopherol, Beta-sitosterol, azulene, valence, Azulene and beta-Panasinen. However, the lowest binding affinity value was obtained from the cytosterol compound of −9.45 kcal/mol in ethyl acetate and Valencene solutions of −6.93 kcal/mol in n-hexane solvent. While the positive control-Chloramphenicol was −36.93 kcal/mol. This means that the syzygium polyanthum leaf extract could be used as an alternative medicine for typhoid.
 GRAPHICAL ABSTRACT

Spectroscopic investigation of preferential solvation of N-confused tetraphenylporphyrinin binary mixtures of dichloromethane with organic cosolvents

Spectroscopic behaviour of porphyrin is known to be sensitive to the choice of the solvent and has been used to probe solvation phenomena. The UV–visible spectra of N-confused tetraphenylporphyrin are observed in a series of binary solvent mixtures – (dichloromethane + diethyl ether), (dichloromethane + chlorobenzene) and (dichloromethane + ethyl acetate). The resulting ET scale for NCTPP solvation indicates nonlinear behaviour and preferential solvation by a solvent–solvent complex in all the three solvents – with the dichloromethane + ethyl acetate system showing the largest deviation from ideality. The data is fitted to the model based on solvent exchange equilibria for determining the preferential solvation parameters which are specific to the probe as well as the identity of solvents in the binary mixture. Further analysis using polarity parameters from literature indicate that the solvation of NCTPP in the (dichloromethane + ethyl acetate) mixture is dependent on the hydrogen bond accepting capacity and polarizability of the medium. Excess spectra derived from ATR-FTIR measurement of dichloromethane + ethyl acetate solutions lead to important inferences about the structure and role of solvent–solvent interactions responsible for the preferential solvation.

Customized Orthogonal Solvent System with Various Hole-Transporting Polymers for Highly Reproducible Solution-Processable Organic Light-Emitting Diodes.

Recently, various hosts and emitters for solution-processable thermally activated delayed fluorescence organic light-emitting diodes (TADF-OLEDs) have been developed. However, a few studies have been conducted on hole transport materials (HTMs) with differentiated solubility characteristics for manufacturing multilayer OLEDs using a solution process. Here, three new hole transport (HT) styrene polymers, PICz, PPBCz, and PTPCz, were synthesized by radical polymerization. Each of the polymers exhibited increases in their highest occupied molecular orbital (HOMO) levels and better hole-transporting abilities than poly(9-vinylcarbazole) (PVK) as a reference HT polymer. Furthermore, the three HT polymers exhibited different solubilities in toluene. Therefore, it was not possible to use a toluene solution to prepare the emitting layer (EML). To overcome this problem, ethyl acetate (EA), in which the three HT polymers are insoluble, was used as an orthogonal solvent to prepare an EML solution. In EA-solution-processed green-emitting TADF-OLEDs, the three HT-polymer-based devices displayed somewhat low turn-on voltages of 2.8 V and high external quantum efficiencies (EQEs) of >23%. These values are superior to those of a device with a PVK-HT layer. In addition, the devices manufactured with the EA solution showed high-performance reproducibility owing to the stable formation of each layer. In this study, we removed the HTM solubility constraint by dramatically changing the solvent for preparing the EML solution and provided an efficient strategy for the fabrication of OLED devices via solution processes in the future.

(Digital Presentation) Power-Generation and Mass-Transport Characteristics of Direct Formic Acid Fuel Cell Using Pore-Designed Anode Electrode

Controlling of mass transport in the anode catalyst layer has become one of the major challenges in Direct Formic Acid Fuel Cells (DFAFCs) owing to the poor formic acid transport and crossover. This study is aim to introduce the microfiber-pores designed anode catalyst layers by mean to improve the mass transport limitation and eventually improving the performance of DFAFCs. Polystyrene fibers (PSFs) were fabricated with different diameter by electrospinning prior to control their length by ultrasonic homogenization. Different amount of PSF as a pore forming agent were then added to the catalyst ink before catalyst coated membrane (CCM) were made by spraying the catalyst ink on the membrane. The CCM were then soaked in ethyl acetate solution to remove the PSF in order to improve the porous structure of anode catalyst layer. Different diameter and amount of PSFs exhibited different pore properties of the catalyst layer and its effect on the mass transport and the performance of DFAFC were then investigated. From the results, the microfiber-pores designed anode catalyst layers showed better performance remarkably at the higher current density region as compared to the conventional anode catalyst layer. Moreover, it was also found that there were optimum diameter and amount of PSF used for the highest performance of DFAFC. This could be attributed to the existence of the microfiber-pores have provide larger active catalyst region which accelerate the fuel transport and the CO2 emission in anode catalyst layer. Thus, these results indicate that the introduction of the microfiber-pores on the anode catalyst layer is a promising approach in order to improve the mass transport resistance, leading to enhance the DFAFCs performance.

Tunable Synthesis of Hydrogel Microfibers via Interfacial Tetrazine Ligation.

Crosslinked, degradable, and cell-adhesive hydrogel microfibers were synthesized via interfacial polymerization employing tetrazine ligation, an exceptionally fast bioorthogonal reaction between strained trans-cyclooctene (TCO) and s-tetrazine (Tz). A hydrophobic trisTCO crosslinker and homo-difunctional poly(ethylene glycol) (PEG)-based macromers with the tetrazine group conjugated to PEG via a stable carbamate (PEG-bisTz1) bond or a labile hydrazone (PEG-bisTz2) linkage were synthesized. After laying an ethyl acetate solution of trisTCO over an aqueous solution of bisTz macromers, mechanically robust microfibers were continuously pulled from the oil-water interface. The resultant microfibers exhibited comparable mechanical and thermal properties but different aqueous stability. Combining PEG-bisTz2 and PEG-bisTz3 with a dangling arginine-glycine-aspartic acid (RGD) peptide in the aqueous phase yielded degradable fibers that supported the attachment and growth of primary vocal fold fibroblasts. The degradable and cell-adhesive hydrogel microfibers are expected to find utility in a wide array of tissue engineering applications.

Spin-casting of Micron-Scale Thick PMMA Films with Embedded Au Nanoparticles Formed by Laser Ablation in Liquid

Background: A Facile, scalable approach to fabrication of organic thin films with an embedded layer of nanoparticles in the ambient environment. The approach is based on step-bystep spin-coating of polymethylmethacrylate (PMMA) films and a nanoparticle layer. Objective: The goal of the present work is to fabricate a sandwich structure of the PMMA films for the top and bottom layers of a sandwich structure as well as a middle layer of nanoparticles formed in solution by the Laser Ablation in Liquid (LAL) method. Methods: First, a PMMA thin film was fabricated by spin-casting of PMMA solution in ethylacetate. Secondly, a solution of Au nanoparticles synthesized by laser ablation in ethanol was spin-cast on a prefabricated PMMA film. The distribution of Au nanoparticles and the morphology of the resulting film were analyzed using scanning electron microscopy (SEM), optical microscopy, and atomic microscopy (AFM). Finally, another PMMA layer was spin-cast on the nanoparticle-decorated film. Results: A hybrid organic film with the embedded layer of nanoparticles was fabricated using the spin-casting method for top and bottom layers as well as for the middle layer of Au nanoparticles fabricated by laser ablation in ethanol by a pulsed UV laser. Statistical and fractal analysis shows uniform distribution of nanoparticles on length scale above ten microns. Conclusion: Spin-cast-based layer-by-layer approach to fabrication of sandwich structures of organic films with embedded nanoparticlesis a facile and scalable method for hybrid organic - nanoparticle films. This approach can be extended for the fabrication of multi-layered hybrid structures.

Method development and optimisation for analysis of pesticide residues in biological matrices by modified QuEChERS and gas chromatography–triple quadrupole mass spectrometry

ABSTRACT A rapid and precise modified QuEChERS method for extraction was developed for simultaneous quantitation of multi-class pesticide residues in human biological matrices, viz. blood, serum and urine. In the modified QuEChERS method, targeted analytes in biological sample were extracted using acidified solution of acetonitrile and ethyl acetate along with anhydrous MgSO4. The collected aqueous layer was evaporated and dispersive solid-phase extraction clean-up was performed. The pesticide residues were assessed using gas chromatography–tandem mass spectrometry with multiple reaction monitoring mode. The developed method was validated as per European Union SANTE/12682/2019 guidelines and the evaluated method validation parameters, viz. linearity, limit of detection, limit of quantitation, accuracy, %relative standard deviation and matrix effect were found to be satisfactory. The proposed method is easy, comprehensible and efficient for simultaneous analysis of diverse range of pesticide residues within similar class. Hence, the present solitary method can be used for systematic analysis of biological samples.

Design of Experiment (DOE) for Optimization of PLGA Nanoparticles

AbstractDesign of Experiments (DOE) is useful tool for formulation optimization. In present study, Design Expert® software (version 13) was used for optimization of Poly(dl‐lactide‐co‐glycolide) (50:50) (PLGA) nanoparticles (NPs). Capecitabine, an approved anticancer drug with short half‐life, was used as model drug. Capecitabine NPs can minimize dosing frequency and improve patient compliance. Effect of two numeric (drug and polymer amount) and one categoric factor (pH of W2 phase) was studied on NP Size and Entrapment Efficiency (EE). Drug amount and pH significantly influenced EE. Polymer amount significantly influenced NP size.MethodsPLGA NPs were prepared by double emulsion technique. Aqueous drug solution (W1) was emulsified with polymer solution in ethyl acetate using probe sonicator (Misonix) for 2 minutes. Formed primary emulsion was sonicated with second aqueous phase (W2) containing stabilizer Kolliphor®P188 for 1 minute to produce double emulsion. Organic solvent and excess water were evaporated at 600 rpm, 60°C for 1.5 hr and NPs were washed thrice (14,000 rpm, 4°C for 45 min) Lyophilized NPs were sonicated with acetonitrile for 5 min and EE was analyzed using UV/Vis spectrometer at ʎmax304nm. Particle size was determined using Malvern Nano‐ZS.ResultsExperimental data were fitted into models of increasing polynomial complexity. EE data is best described by two‐factor interaction model with R² of 0.9145. ANOVA results show model is significant. Predicted R²of 0.8076 is in reasonable agreement with adjusted R² of 0.8824. Drug amount, pH of W2 phase and their interaction are significant (p<0.05). Higher drug amount decreases EE which maybe because polymer amount was not sufficient to encapsulate increased drug amount and more drug migrated to W2 phase. Lower EE at pH 4.5 might be described by drug leaching into W2 phase due to better drug solubility. Diagnostic normal plot, perturbation plots, interaction plots and 3D‐surface plot confirm model robustness. Size data was best fitted to linear model showing polymer amount being significant. Higher polymer amount might have decreased dispersion efficiency of first emulsion into W2 phase and led to fusion of semi‐formed particles to larger size.Numerical OptimizationThe desired goals were set to minimize polymer amount (to increase drug amount per unit weight of NPs), to minimize drug amount and the pH was set at 7.4 to maximize EE. Predicted optimum responses were checked experimentally. Batch prepared with 120mg polymer and 25mg capecitabine has average size of 111.3 nm (predicted value 116.8nm) and EE of 38% (predicted value 40%), both with 5% coefficient of variance.ConclusionDOE gives an opportunity to look at individual and combined impact of various factors. It can provide valid conclusions with minimal experimental runs, time, and cost. Similar DOE approaches can be used for other PLGA‐drug formulations optimization.Conflict of InterestAuthors declare no conflicts of interest.

Calcium Decay Ability of Extracts Chromolaena odorata L. Leaves (Asteraceae) on Kidney Stones

Background: Kidney stones are one of the causes of chronic and acute kidney failure symptoms. The flavonoid compounds in Chromolaena odorata leave extract are thought to dissolve calcium in kidney stones. Objective: This study aims to determine the activity of Chromolaena odorata leaves extract as a laxative for calcium kidney stones and to characterize the active extract with a liquid chromatograph mass spectrometry. Methods: The leaves of Chromolaena odorata were extracted by ultrasonication method using 3 solvents in stages, namely n-hexane, ethyl acetate, and methanol. The powder for kidney stones was immersed in an extract solution of n-hexane, ethyl acetate, and methanol for 5 hours at 37° C. The reaction results were analyzed for their absorbance using a UV-Vis spectrophotometer. The fraction with the best activity was analyzed for phytochemical content with various typical reagents and LCMS. Results: Methanol extract of Chromolaena odorata has a better effect in dissolving calcium kidney stones. Methanol extract of Chromolaena odorata can reduce calcium in kidney stones with an EC50 value of 16801 µg/mL. Based on phytochemical tests and LCMS analysis, the methanol extract of Chromolaena odorata leaves contains compounds of the tannins, alkaloids, flavonoids, and steroids. Chromatogram at a retention time of 7.76; 8.96; and 10.01 in the methanol extract of Chromolaena odorata identified 3,5,7,4'-tetrahydroxy-8,3'-dimethoxyflavone; 5,7,4’-trihydroxy-3’,5’-dimethoxyflavone, and 5,6,7,8,4'-pentamethoxyflavone compounds. Conclusion: Methanol extract had the best calcium decay activity in kidney stones with an EC50 value of 16801 µg/mL. 3,5,7,4'-tetrahydroxy-8,3'-dimethoxyflavone; 5,7,4’-trihydroxy-3’,5’-dimethoxyflavone, and 5,6,7,8,4'-pentamethoxyflavone compounds are contained in methanol extract which is thought to play a role in shedding calcium in kidney stones.

Dip-and-Read, Organic Solvent-Compatible, Paper-Based Analytical Devices Equipped with Chromatographic Separation for Indole Analysis in Shrimp.

We developed an organic solvent-compatible paper-based analytical device (PAD) for the quantitative analysis of indole, which is an indicator of shrimp freshness. Although indole is insoluble in water, ethyl acetate is a suitable solvent to dissolve and extract indole from shrimp. The PADs are fabricated using a cutting method that allows the use of an organic solvent because no hydrophobic barrier is needed to form fluidic channels. Ehrlich's reagent consists of 4-(dimethylamino)benzaldehyde and p-dimethylaminobenzaldehyde and was deposited onto the reaction zone of the PAD followed by lamination to prevent evaporation of the ethyl acetate. Samples are introduced into the PAD via immersion in organic sample solutions. When the PAD is immersed into an indole solution of ethyl acetate in a closed bottle, the sample solution penetrates the channel of the PAD and successively flows into the detection zone to form a hydrophilic colored product. The PADs provide a linear relationship between the logarithm of the indole concentration and the color intensity within a range of 1.0-20 ppm with correlation coefficients of r2 > 0.99. The limits of detection and quantification are 0.36 and 0.71 ppm, respectively. Relative standard deviations for both the intraday (n = 2) and interday (n = 3) precision were less than 2.5%. In the indole analysis of shrimp, the PADs separated the interfering orange-colored astaxanthin in the extract from the colored product of indole via the paper chromatographic principle. We used the PADs to investigate the degradation of shrimp, and the results showed a rapid increase in the indole level after 7 days. High-performance liquid chromatography verified the accuracy of the PADs by showing good agreement with the obtained indole levels.

Indonesian Ciplukan Extract Inhibited TGF-β1/NF-κB Pathway in Experimental Psoriasis Mouse Models

Background:The global prevalence of psoriasis, a chronic inflammatory skin disease, has substantially increased in the last decade. The increase activity of Transforming Growth Factor ß1 (TGFß1)/nuclear factor kappa-light-chain-enhancer of activated B cells (NF-κB) pathway which cause inflammation, is the major pathological mechanism in psoriasis. Current psoriasis treatment using chemical agents is hampered by the side-effects when used long-term, which underlines the need for alternative, low side-effect anti-psoriatic agents. The extract of Physalis angulata L., also known as Ciplukan in Indonesia, contains Physalins, compounds known for their anti-inflammatory effects, but whose effect on psoriasis has not been studied.
 Objective: This study aimed to investigate the effect of Ciplukan extract (CE) to TGFß1/NF-κB pathway in psoriasis mouse models.
 Methods: This was experimental study with posttest-only control group design. The CE active ingredients were identified using Liquid chromatography-tandem mass spectrometry (LC-MS/MS). Twenty-five female imiquimod (IMQ) induced psoriasis-like dermatitis mice were allocated into five groups, with three groups receiving 7 days of 400, 800, and 1200 mg/kg bodyweight doses of CE, respectively, and two groups serving as control and IMQ groups. The NF-κB and TGFß1 expressions were evaluated using Allred score based on immunohistochemistry (IHC) staining. Histopathology and clinical psoriasis manifestations were assessed using Baker’s from Hematoxylin Eosin (HE) staining and Psoriasis Area Severity Index (PASI) scores. The Kruskal-Wallis followed by Mann Whitney tests were conducted for data analysis. The p-value < 0.05 was considered to be statistically different. 
 Results: Based on LC-MS/MS test, Physalin B, D, and F were active ingredients from CE in ethyl acetate solution. An improvement in psoriasis inflammation was observed in 400 and 800 mg/kg bodyweight doses of CE, but only the dosage of 800 mg/kg BW significantly decreased of Allred scores from NF-κB and TGFß1 expressions; Baker’s and PASI scores compared to IMQ group (p<0.05). The 1200 mg/kg bodyweight doses of CE associated with acute toxicity signs and mortality, meanwhile dosage of 800 mg/kg BW showed the highest efficacy with lowest toxicity effect.
 Conclusions: Ciplukan extract improved psoriasis manifestations via inhibition effect to TGFß1/NF-κB pathway and the extract might be developed as an alternative anti-psoriasis agent

Concentration dependency of dispersion coefficient of aqueous solutions of urea and ethyl acetate in porous media

AbstractWe report new measurements of the concentration‐dependent longitudinal dispersion coefficient of aqueous urea and ethyl acetate solutions in a porous medium at a wide range of concentrations. The longitudinal dispersion coefficient was obtained by injection of a pulse of an aqueous solution of urea (or ethyl acetate) into a carrier phase flowing through a porous column and analysis of the effluent peak using the Taylor dispersion theory. The measured longitudinal dispersion coefficients for different velocities and concentrations showed an increasing trend with concentration and pore velocity. The longitudinal dispersion coefficient measurements show a power‐law relationship with the Peclet number . The results are compared with experimental data and empirical formulas available in the literature, and a reasonable agreement is achieved over the range of Peclet numbers studied.

1-(Methyl-α-d-gluco-pyran-osid-6-yl)-3-vinyl-imidazolium iodide di-methyl-formamide monosolvate.

The title solvated molecular salt, [MeGluVIm]I (MeGluVIm = 1-(methyl-α-d-gluco-pyran-osid-6-yl)-3-vinyl-imidazolium), or C12H19N2O5 +·I-·C3H7NO, was synthesized from methyl-α-d-6-iodo-gluco-pyran-oside and vinyl-imidazole in DMF. It crystallizes through precipitation from ethyl acetate solution directly after the reaction procedure. The crystal structure consists of an iodide anion and a [MeGluVIm] cation. Furthermore, the crystal structure contains one mol-ecule of DMF, which accepts two O-H⋯H hydrogen bonds from the OH groups of the gluco-pyran-oside.