Synthesis, characterization and biological activity of Pyrazoline derivatives

Pyrazoline is dihydropyrazole having only one endocyclic double bond. Synthesis of pyrazoline derivatives from chalcones is an active arena of investigation due to established pharmacological result. In present study, chalcones were prepared by reacting of acetophenone with benzaldehyde. Then prepared chalcones react with isoniazid in the presence of glacial acetic acid results pyrazoline derivative. Physical parameters such as color, crystal structure, solubility, melting point, retardation factor (Rf) and % yield was evaluated. Confirmations of structures of all synthesized derivatives, were done by spectroscopic data of IR, 1HNMR and Mass spectroscopy. Also, all synthesized compounds were evaluated for antibacterial activity against B. subtilis, S. aureus, P.aeruginosa and E.coli, and antifungal activity was accomplished against C. albicans and A. niger at the different conc. and concluded that some compounds have excellent antimicrobial activity and most of the synthesized compounds exhibits moderate antimicrobial activity.

Assessment of The Dioxins Leaching Potentials In Selected Soils Through Breakthrough Curves (BTCs) Model

The current study was to investigate the leaching and groundwater contamination potential of selected Dioxins, in local soil series. Solute transport was modelled through Breakthrough curve (BTC) plots, based on distribution coefficient (Kd), Retardation factor and Dispersivity, under normal velocity (20 cm day -1) and preferential or steady flow (50 cm day -1). In case of Dibenzo -p- Dioxin (DD), distribution coefficient values were found in order of Charsadda > Peshawar > Sultanpur series, while for 2 Chloro- p- Dioxin (2Cl-DD), the order was Charsadda > Sultanpur > Peshawar. However, the overall sorption was low. Under the normal velocity both of selected Dioxins (DD & 2Cl-DD), BTC plots relatively took longer time to reach the point of saturation as compared to high seepage velocity. However, the overall solute transport was found to be rapid. This behaviour showed that sorption of the Dioxins selected soil series is low and there is potential for leaching and groundwater contamination.

An Application of Safety Assessment for Radioactive Waste Repository: Non-Equilibrium Transport of Tritium, Selenium, and Cesium in Crushed Granite with Different Path Lengths

Advection-dispersion experiments (ADE) were effectively designed for inadequate transport models through a calibration/validation process. HTO, selenium (Se), and cesium (Cs) transport in crushed granite were studied using a highly reliable, dynamic column device in order to obtain the retardation factors (R) and the dispersion coefficients (D) by fitting experimental breakthrough curves (BTCs) for various path lengths. In order to conduct a safety assessment (SA) of a deep geological repository for high-level radioactive waste, radionuclide transport in rock systems is necessary to clarify and establish a suitable model. A dynamic column with a radiotracer (HTO, Se(IV), and Cs) was applied to 2, 4, and 8 cm path lengths using a STANMOD simulation. The results showed similar results between the BTCs of Se and Cs by fitting a non-equilibrium sorption model due to the retardation effect. In fact, there was a relatively obvious sorption of Se and Cs in the BTCs obtained by fitting a retardation factor (R) value higher than 1. In addition, a two-region (physical) and a two-site (chemical) non-equilibrium model with either the lowest sum of squared residuals (SSQ) or the root mean square error (RMSE) were applied to determine the Se and Cs sorption mechanisms on granite.

Exploring the conservativeness of deuterated water as the artificial tracer for hydrogeological tests

Deuterated water has been applied in hydrogeological tracer tests in recent years. However, there is a contradiction about the conservativeness of artificial deuterium (D/2H). In this study, what circumstances HDO behaved truly conservatively were investigated through laboratory-scale experiments via comparing the widely used tracer chloride (Cl-). And reasons for the non-conservativeness of HDO were discussed comprehensively for the first time. In addition, the advection-dispersion equation (ADE) and dual-domain mass transfer (DDMT) equation were employed to describe the breakthrough curves (BTCs) of tracers. HDO behaved conservatively when it transported in the porous media with high permeability (approximately K > 1m/d), and ADE could describe BTCs successfully. While hysteresis effect of HDO expressed in the media with low permeability. And the lower the permeability of the porous media, the stronger the hysteresis effect. DDMT was more suitable for demonstrating BTCs in low permeability media. Hydrogen bonds between HDO and H2O, the isotopic exchange effect, and the dual-domain model of the media all could lead to the hysteresis effect. The retardation factor (R = 1.712) was used to describe transporting behaviors of HDO in clay firstly. And the threshold hydraulic conductivity (Kcr) and the proportion of immobile regions of HDO were greater than that of Cl-, while dispersion coefficients of HDO were smaller. These could provide further considerations for using deuterium in hydrogeological tracer tests.

Supercritical Carbon Dioxide Extracts of Cordyceps sinensis: Chromatography-based Metabolite Profiling and Protective Efficacy Against Hypobaric Hypoxia

The toxicity and disposal concerns of organic solvents used in conventional extraction purposes has entailed the need for greener alternatives. Among such techniques, supercritical fluid extraction (SFE) has gained popularity by yielding extracts of high purity in a much faster manner. Carbon dioxide (CO2) is generally preferred as a supercritical solvent because of its lower temperature requirements, better diffusivity and easy removal. The present study describes the characterization of supercritical CO2 extracts of Indian variety of Cordyceps sinensis (CS)- a high-altitude medicinal mushroom widely revered in traditional medicine for its extensive anti-hypercholesterolemic, anti-inflammatory, anti-proliferative and energy-enhancing properties. Experimental parameters viz. 300 and 350 bar of extraction pressure, 60°C of temperature, 0.4°L/h CO2 of flow rate and use of 1% (v/v) of ethanol as entrainer were optimized to prepare three different extracts namely, CSF1, CSF2 and CSF3. High-performance thin-layer chromatography (HPTLC) was used for assessing the quality of all the extracts in terms of cordycepin, the pivot biomarker compound in CS. Characterization by HPTLC and GC-MS confirmed the presence of flavonoids and nucleobases and, volatile organic compounds (VOCs), respectively. The chromatographic data acquired from metabolite profiling were subjected to chemometric analysis in an open source R studio which illustrated interrelatedness between CSF1 and CSF2 in terms of two major principal components. i.e. Dim 1 and Dim 2 whose values were 40.33 and 30.52% in variables factor map plotted using the HPTLC-generated retardation factor values. The factor maps based on retention times of the VOCs exhibited a variance of Dim 1 = 43.95% and Dim 2 = 24.85%. Furthermore, the extracts demonstrated appreciable antibacterial activity against Escherichia coli and Salmonella typhi by generation of reactive oxygen species (ROS), protein leakage and efflux pump inhibition within bacterial pathogens. CSFs were elucidated to be significantly cytoprotective (p < 0.05) in a simulated hypobaric hypoxia milieu (0.5% oxygen). CSF2 showed the best results by effectively improving the viability of human embryonic kidney (HEK 293) cells to 82.36 ± 1.76% at an optimum dose of 100 µg/ml. Levels of hypoxia inducible factor-1 alpha (HIF-1α) were modulated four-fold upon supplementation with CSF2. The results collectively evinced that the CSF extracts are substantially bioactive and could be effectively utilized as mycotherapeutics for multiple bioeffects.

Distribution of Uranium Isotopes in Sandy Deposits by Sequential Extraction

The sequential extraction procedure is used to reconstruct the processes of redistribution of uranium isotopes in the mineral phases of the aquifer of the Vendian sandy-argillaceous deposits developed in the coastal territory of the European North of Russia. This aquifer has large resources of drinking and mineral groundwater which, however, are used in extremely limited quantities. This is due to the very complex nature of the hydrochemical conditions, and uranium-isotopic methods are used to clarify these conditions. The following mineral phases of core samples were characterized: adsorbed trace materials and carbonate minerals; ferrihydrate, amorphous minerals of Fe, Al and Si, and secondary U minerals; crystalline iron minerals; clay and some refractory minerals; and all remaining resistant minerals. The most resistant minerals, whose fraction ranges from 70.58 to 96.4%, have a minimum average uranium concentration of 0.47 ppm. This uranium is practically conserved in the rock, as a result of which the average ratio of its 234U:238U isotopes is close to equilibrium. In the remaining fractions, uranium is redistributed by groundwater along their flow lines from recharge areas in watersheds to areas of discharge into river valleys. Its maximum concentration (12.89 ppm) measurement is carried out by coprecipitation with iron hydroxides, then the uranium is adsorbed and precipitated with carbonates (9.14 ppm). The average 234U:238U is maximum in adsorbed trace materials and carbonate minerals (2.39 ± 0.36) and is close to that in fresh groundwater (2.8 ± 0.42). It is also increased in the amorphous minerals of Fe (1.53 ± 0.23). In general, there is a dependence of the 234U:238U activity ratio in rock on the degree of participation of groundwater in the deposition of hydrogenic uranium isotopes into the cracks and pores of these rocks. The results obtained contribute to the refinement of such a parameter as the retardation factor, which is necessary for understanding the processes of migration and concentration of uranium in sedimentary basins.

The extended transfer function model for the simulation of pesticides transport along the unsaturated zone

<p><span lang="EN-US">The scope of this work is to present the extended transfer function model (TFM-ext) that allows to simulate the spatio-temporal distribution of nonpoint-source pollutants, e.g., pesticides, along the unsaturated zone, till the groundwater table depth.</span></p> <p><span lang="EN-US">The model is based on the transfer functions approach, i.e., on the travel time probability density functions (TT pdfs), which describe the leaching behavior in a given soil profile. The strength of the model, despite the important assumptions on time-invariant TT pdfs and steady-state input fluxes, is that it derives the TT pdfs from a physical quantity, i.e., the unsaturated hydraulic conductivity function k(</span>θ<span lang="EN-US">).  Moreover, the model extends the transport process to the generic depth z, where information on hydraulic properties could not be available, assuming a lognormal travel time pdf, whose parameters are scaled according to the generalized transfer function model. </span><span lang="EN-GB">In the case of reactive solutes, the model considers both the mass decay and the retardation factor.</span></p> <p><span lang="EN-US">The TFM-ext was validated in Valle Telesina, a hilly area of around 200 km<sup>2</sup><span class="apple-converted-space"> </span>in Italy. Forty-six soil profiles, completely characterized from the hydrological point of view, were used to evaluate the mean travel times and the breakthrough curves at the groundwater depth and then compared with the results of a physically based model, Hydrus 1D. Results gave very high correlation coefficients (above 0.8), a mean absolute error of around 40 days and a percent bias of -16%.</span></p> <p><span lang="EN-US">Moreover, a comprehensive sensitivity analysis to evaluate to which parameters the TFM-ext is more sensitive, was performed. Results shown that </span>τ <span lang="EN-US">anf θ<sub>s</sub> parameters related to the slope of the k(θ) are those affecting more the travel time. </span></p> <p><span lang="EN-US">The model was implemented as an operative tool for the specific groundwater vulnerability assessment within the geospatial Decision Support System developed for LANDSUPPORT H2020 project.</span></p>

Implementation of Two Chromatographic Methods for Simultaneous Quantitation of Thioctic Acid, Benfotiamine and Cyanocobalamin

Two accurate and sensitive chromatographic methods have been introduced and validated for the simultaneous determination of thioctic acid, benfotiamine and cyanocobalamin in bulk powders and in their pharmaceutical formulation. Method A is reversed-phase ultra performance liquid chromatographic method with an isocratic elution, where a rapid separation was accomplished on a Zorbax C8 column using a mobile phase of acetonitrile:0.05 M phosphate buffer (pH 6 adjusted by o-phosphoric acid) (23:77, v/v). The retention times (tR) were 0.578, 0.852 and 1.376 for cyanocobalamin, benfotiamine and thioctic acid, respectively. The separated peaks were revealed at 210.0 nm. Method B is a thin-layer densitometric method where the separation of the studied drugs was carried out on silica gel plates using methanol–chloroform–heptane-1-sulphonic acid sodium salt (0.4%) (7:3:0.1, by volume) as a mobile phase, and scanning of the separated bands was done at 240.0 nm. The retardation factor (Rf) values were 0.17, 0.48 and 0.75 for cyanocobalamin, benfotiamine and thioctic acid, respectively. Validation of the methods was achieved following ICH guidelines and the applied methods succeeded to determine the cited drugs in their pure forms and capsules. Results were statistically compared to the manufacturer’s method where no significant difference was observed.

PENGEMBANGAN DAN VALIDASI METODE AKRILAMIDA PADA UBI JALAR GORENG SECARA KROMATOGRAFI LAPIS TIPIS-DENSITOMETRI

Penelitian ini dilakukan karena sebelumnya belum ada laporan tentang metode kromatografi lapis tipis (KLT) Densitometri untuk analisis akrilamida dalam ubi jalar goreng. Hasil penelitian menggunakan lempeng KLT silika gel 254 menunjukkan bahwa retardation factor berkisar 0,4-0,5 dengan eluen metanol: benzena (2:1) dan dianalisis di panjang gelombang maksimum 200 nm. Linieritas standar akrilamida diuji dalam rentang konsentrasi 120-300 ppm dan koefisien korelasi (r) lebih besar dari 0,99, dengan batas deteksi 17,45 ppm dan batas kuantitatif 52,36 ppm. Persiapan sampel dilakukan dengan cara ekstraksi pelarut menggunakan etanol 70%. Presisi memberikan hasil 2,67% dan nilainya lebih kecil dari 16% sesuai literatur. Persen recorvery 98,18% dan sesuai dengan literature yaitu 98% -102%. Dari penelitian ini dapat disimpulkan bahwa metode KLT Densitometri pada penentuan akrilamida selektif, presisi, dan akurat dimana pada penetapan kadar akrilamida pada ubi jalar goreng mengandung akrilamida sangat sedikit dimana konsentrasinya kurang dari 230,32 ng sehingga sampel ini sangat aman untuk dikonsumsi.

Simulation of reactive solute transport in the critical zone: a Lagrangian model for transient flow and preferential transport

We present a method to simulate fluid flow with reactive solute transport in structured, partially saturated soils using a Lagrangian perspective. In this context, we extend the scope of the Lagrangian Soil Water and Solute Transport Model (LAST) (Sternagel et al., 2019) by implementing vertically variable, non-linear sorption and first-order degradation processes during transport of reactive substances through a partially saturated soil matrix and macropores. For sorption, we develop an explicit mass transfer approach based on Freundlich isotherms because the common method of using a retardation factor is not applicable in the particle-based approach of LAST. The reactive transport method is tested against data of plot- and field-scale irrigation experiments with the herbicides isoproturon and flufenacet at different flow conditions over various periods. Simulations with HYDRUS 1-D serve as an additional benchmark. At the plot scale, both models show equal performance at a matrix-flow-dominated site, but LAST better matches indicators of preferential flow at a macropore-flow-dominated site. Furthermore, LAST successfully simulates the effects of adsorption and degradation on the breakthrough behaviour of flufenacet with preferential leaching and remobilization. The results demonstrate the feasibility of the method to simulate reactive solute transport in a Lagrangian framework and highlight the advantage of the particle-based approach and the structural macropore domain to simulate solute transport as well as to cope with preferential bypassing of topsoil and subsequent re-infiltration into the subsoil matrix.