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Acta Chromatographica
Authors:
Luis Alejandro Pérez-López
,
Norma Cavazos-Rocha
,
Cecilia Delgado-Montemayor
,
Noemí Waksman-Minsky
,
Marcelo Hernández-Salazar
, and
Omar J. Portillo-Castillo

Abstract

The analysis of phenolic acids (PAs) is of great importance, because they are frequently present in natural products and their derivatives, and these compounds also have multiple beneficial effects to human health. This work is focusing on the separation of seven PAs (caffeic acid, coumaric acid, gallic acid, ferulic acid, protocatechuic acid, sinapic acid, and syringic acid), in a reversed-phase liquid chromatographic (RP-HPLC) isocratic method using a hydrophilic deep eutectic solvent (DES) as a mobile phase additive. The analysis was carried out with a diode array detector. The used DES was composed by choline chloride and glycerol, and it was characterized by infrared spectroscopy. The combination of choline chloride:glycerol (1:4) added at 0.25% to mobile phase composed of 0.15% formic acid aqueous solution and methanol (80:20), showed the best separation for target analytes. The new proposed method was validated, and results indicated that the proposed method is linear, selective for almost all analytes, provided high sensitivity with limit of detection ranges from 0.009 to 0.023 mg mL−1, and has satisfactory precision and accuracy, with values of relative standard deviation of 0.24–2.65% and recoveries of 97.97–109%, respectively. Additionally, this method was successfully applied to simultaneous determination of phenolic acids in three kinds of samples of powder to prepare lemon flavour drink enriched with black tea extract.

Open access

Abstract

Dendrobium nobile and Dendrobium officinale as the main varieties of traditional Chinese medicine Dendrobium are widely used in clinic. The study aimed to systematically explore chemical constituents and their antitumor effect of D. nobile and D. officinale by ultra-performance liquid chromatography coupled with ion trap time-of-flight mass spectrometry (UPLC-IT-TOF), network pharmacology and cancer cell experiments. D. nobile extract and D. officinale extract could significantly inhibit the proliferation of human lung cancer A549 cells, human liver cancer HepG2 cells and human breast cancer MCF-7 cells in the dose-dependent manner (P < 0.05), the antitumor effect of D. officinale extract was stronger than that of D. nobile extract at the same drug concentration. A total of 40 chemical constituents of D. nobile and D. officinale including phenanthrenes, bibenzyls and other types of compounds had been identified by UPLC-IT-TOF, LCMSsolution and MetID software according to retention times, accurate mass, MSn fragmentation, reference compounds and natural product databases. Phenanthrenes with good antitumor activity were mainly present in D. nobile, bibenzyls were the main compounds of D. officinale. Integrated networks of Herb-Compounds-Targets-Cancer revealed that gigantol, moscatilin, tristin, moscatin and densiflorol B were regarded as key antitumor compounds of D. nobile and D. officinale, D. nobile and D. officinale shared 7 targets accounting for 70% of the antitumor core targets, more than half of their antitumor KEGG pathways were similar. The results of molecular docking and western blotting experiments indicated that the antitumor mechanisms of D. nobile and D. officinale may be through inhibiting PI3K-Akt and HIF-1α signaling pathways.

Open access

Cover crops serve as an essential source of nutrients in the soil and generally improve the soil’s properties. Cover crops’ production is considered a benefit of the soil quality; by protecting the soil from erosion, reducing the weeds and the so-called soil-borne plant pathogens. Different varieties of cover crops can be cultivated such as legumes, non-legumes, brassica, and grass-type of plants with a variability of the symbiosis. A pot experiment was carried out with five cover crops, as non-symbiont (Brassica carinata B.c.), single-symbiont with arbuscular mycorrhiza fungi (AMF) (Phacelia tanacetifolia P.t., Avena strigosa A.s.) and double symbiont with AMF and nitrogen-fixing bacteria (Vicia benghalensis V.b., Vicia faba V.f.) crops; and a mixture of the five species, placed in sandy soil (arenosol) in plastic pots (5000 g soil) in 4 repetitions. One of the pots with mixed cover crops was inoculated by AM fungi industrial product. We measured soil biological activity of dehydrogenase (DHA) and fluorescein-diacetate (FDA) enzymes, the frequency of AM fungi (F%), the all protein, glomalin content and electrical conductivity (EC) of the soils. Mixture of all the cover crops resulted maximum EC and significantly enhanced the enzymatic, DHA, FDA activities in comparison with single plants. Mycorrhiza colonization frequency was high in all cover crops except the mustard (B.c.), as nonsymbiont. Vetch (V.b.), as double symbiont was responding very positively to AMF inoculation, and enhanced the performance of its growth. It was found in the pot experiment, that vetch, has the highest capacity to retain soil-protein, glomalin concentration, as well. The mixture of five cover crops could be suggested to use, due to the synergistic positive performance of the individual crops, and the better functioning of beneficial fungal / bacterial symbiosis.

Open access
Agrokémia és Talajtan
Authors:
László Simon
,
Marianna Makádi
,
Zsuzsanna Uri
,
Szabolcs Vigh
,
Katalin Irinyiné-Oláh
,
György Vincze
, and
Csilla Tóth

Open-field small plot long-term experiment was set up during 2011 with willow (Salix triandra × S. viminalis ‘Inger’), grown as a short rotation coppice energy crop in Nyíregyháza, Hungary. The sandy loam Cambisol with neutral pH was treated three times (2011, 2013, and 2016) with 15 t ha–1 municipal sewage sludge compost (MSSC) and with 600 kg ha–1 (2011, 2013) or 300 kg ha–1 (2016) wood ash (WA). In 2018 the MSSC-treated plots were amended with 7.5 t ha–1 municipal sewage sediment (MSS), and 300 kg ha–1 WA. MSSC and WA or MSS and WA were also applied to the soil in combinations during all treatments. Control plots remained untreated since 2011. Repeated application of wastewater solids (MSSC, MSS) and wood ash (WA) significantly enhanced the amounts of As (up to +287%), Ba, Cd (up to +192%), Cu, Mn, Pb, and Zn in the topsoil of willows. The combined application of MSSC+MSS+WA resulted in significantly higher Mn and Zn and lower As Ba, Cd Cr, and Pb concentrations in topsoil than MSSC+MSS treatment of soil without WA. Nitrogen concentrations in leaves of treated plants were generally slightly lower or similar to control. All soil treatments significantly enhanced the uptake or accumulation of nutrient elements (Ca, K, Mg, P) and potentially toxic elements (As, Ba, Cd, Cr, Cu, Mn, Ni, Pb, and Zn) in the leaves of willows during 2018, 2019, and 2020. Significantly higher Mn or Zn concentrations were measured in MSSC+MSS+WA than in MSSC+MSS treatments. Significant amounts of Cd (up to 1.11 mg kg–1) or Zn (up to 183 mg kg–1) can be translocated (phytoextracted) from a soil amended with wastewater solids or wood ash to willow leaves. In 2018 the treatments decreased the chlorophyll fluorescence values, while in 2019 and 2020 the light adapted fluorescence yield (Y) values were higher in treated than in control plants.

Open access

In this study PTEs, [potentially toxic elements (Cr, Cu, Mn, Ni, Pb, and Zn)] were investigated in the upper layer of floodplain soils that occurred as a result of accident in the area of two mine tailings in Northwestern Romania. A large amount of sediment was deposited on the soil of floodplains along the Hungarian section of River Tisza, which could represent a threat to the environment. Floodplain soil samples were collected from four locations in Hungary from an area of the river stretching to about 250 km. BCR (Bureau Communautaire de Référence) sequential extraction method was used to analyze both post-flood and present samples. Most of the analyzed elements (Cd, Cr, Cu, Ni, Pb, Zn) were found in the residual fraction, but there is a notable soluble amount in hydroxylammonium chloride extractable fraction. The results allow a comparison of the changes that have taken place over time, in addition to serving as a basis for further studies.

Open access

Abstract

As per the World Health Organization, 10% of medicines in low- and middle-income nations are of poor quality and pose a huge public health risk. The development and implementation of cost-effective, efficient and quick analytical methods to control the quality of these medicines is one of the immediate strategies to avoid such a situation. Hence, the main goal of this study was to develop and validate a simple, specific and precise new RP–HPLC method for simultaneous analysis of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations. The chromatographic analysis was achieved using Shodex C18 (250 × 4.6 mm, 5 μm) column with UV detection at 225 nm. The mobile phase was a gradient mixture of 30 mM phosphate buffer, pH 4.0 (mobile phase A) and acetonitrile (mobile phase B). Efficient separation of the three drugs was obtained using the final optimized chromatographic conditions. The developed method was validated for its specificity, linearity, precision, accuracy and robustness as per the ICH guidelines. The validation results showed that the method was specific, linear, precise, accurate and robust for the simultaneous determination of the three drugs. The developed method was applied to determine the content of the three drugs in pharmaceutical formulations. The assay results of the preparations showed that their drug content was within the pharmacopeial limit stipulated for each drug product. It can be concluded that the proposed method is suitable for simultaneous determination of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations in industries and regulatory laboratories.

Open access
Agrokémia és Talajtan
Authors:
Norbert Túri
,
János Körösparti
,
Balázs Kajári
,
György Kerezsi
,
Mohammed Zain
,
János Rakonczai
, and
Csaba Bozán

Due to extreme meteorological and soil hydrological situations the agricultural production security is highly unpredictable. To release the extent and duration of inland excess water (IEW) inundations or two-phase soil conditions during the period intended for cultivation, subsurface drainage (SD) has been used as a best practice in several countries. SD interventions took place between 1960’s and 1990 in Hungary. After 1989, land ownership conditions changed, thus professional operation and the necessary maintenance of the SD networks designed as a complex system became insignificant. In this paper, our aim was to present the IEW hazard in one of the most equipped areas by SD in Hungary. The occurrence frequency of IEW inundations in drained and non-drained (control) areas in different time intervals were compared. According to our results, we could state that the frequency of IEW on the subsurface drained areas was moderately lower in only a few periods compared to the control areas. IEW hazard of the arable areas at the Körös Interfluve was classified as nonhazarded in 52.7% of the area. Another 38.2% were moderately hazarded, 8.26% of the lands were meanly hazarded and less than 1% were highly hazarded area by IEW.

Open access

Abstract

Purpose

Development and validation of a selective analytical method to accurately and precisely quantify nicotine and cotinine levels in rat's plasma after exposure to tobacco cigarettes and tobacco water-pipe.

Methods

An easy HPLC-Photodiode-Array Detection (PDA) method was developed and validated for simultaneous determination of nicotine and cotinine levels in plasma of 15 rats (10 rats after tobacco products exposure and 5 control rats). Nicotine and cotinine were extracted in one step from plasma using acetonitrile and concentrated to lowest volume using nitrogen stream.

Results

The developed method offered a rapid analysis time of 14 min with single step of analytes extraction from rat's plasma with recovery percentage range between 93 and 95% and excellent linearity with correlation factor more than 0.994 with analytical range between 50 and 1000 ng mL−1 and LOD of 25 ng mL−1 and 23 ng mL−1 for nicotine and cotinine, respectively. The analysis of rat's plasma after 28 days of exposure to tobacco cigarettes and tobacco water-pipe revealed that the average concentrations of 376 ng mL−1 for cotinine and 223 ng mL−1 for nicotine were obtained after tobacco cigarettes exposure, and 220 ng mL−1 for cotinine and 192 ng mL−1 for nicotine after tobacco water-pipe exposure.

Conclusion

Higher nicotine and cotinine levels were found in plasma after tobacco cigarettes exposure than water-pipe exposure which may have potential undesirable effects on passive smokers in both cases.

Open access

The Westsik’s long-term crop rotation experiment was set up in 1929 at the Nyíregyháza Experimental Station (NE Hungary) on a slightly acidic Arenosol. Besides fallow crop rotation (CR), effects of different organic amendments (lupine as green manure, lupine as main crop, straw manure, and farmyard manure (FYM) were studied with or without N or NPK-fertilizers. The crop rotation consisted of rye, potato, lupine, and oat with common vetch. The soil of potato plots was analysed in 2019 at the 90th anniversary of Westsik’s crop rotation experiment.

The following chemical and microbiological soil parameters were determined: soil pH, available nutrient contents, organic carbon (OC) and nitrogen (ON) contents, microbial biomass carbon (MBC) and nitrogen (MBN), soil respiration, net nitrification, and activity of some soil enzymes.

In the CRs, the soil pHH2O varied from acidic to weakly alkaline and it largely differed from pHKCl. The results showed a significant increase in the content of nitrate, available phosphorus and potassium in most of the fertilized plots. Applying straw, green manure, or FYM significantly increased the OC and ON contents. The total count of cultivable bacteria increased upon the application of the organic manures. Combined application of straw manure and N-fertilization heavily improved the abundance of the microscopic fungi.

While all the applied organic manures significantly enhanced the MBC, the MBN increased only by the green manure amendment. Our results revealed higher soil respiration rate in the plots receiving straw or FYM than in the control. Both green manure and FYM elevated the net nitrification rate. Phosphatase, saccharase, urease, and dehydrogenase enzymes showed a hesitating response to the manure application in the different CRs.

The soil respiration and dehydrogenase activity correlated to most of the measured chemical parameters. Among microbiological properties, the MBC and MBN, as well as dehydrogenase and other enzyme activities displayed a positive correlation. Results proved the need for the exogenous application of organic matter in the form of organic manures to enhance the nutritional status and health of the soil.

Open access