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Chemical engineering is an engineering branch that deals with the chemical production and manufacture of products that undergo chemical processes. This includes equipment design, creating systems and processes to refine raw material, as well as mixing, compounding, and processing chemicals to create products.
Chemistry and Chemical Engineering
Szarvasmarhatartó telepen alkalmazott ivarzásindukáló hormonok megjelenése a hígtrágyában
Appearance of on-farm bovine reproductive hormones in the resulting slurry
A nemzetközi irodalmat is áttekintve azt találtuk, hogy az intenzív tejelő szarvasmarhatartásban felhasznált ivarzásindukáló hormonkészítmények mennyiségét és a hígtrágyában való megjelenését még nem vizsgálták. Kutatásunkban egy Pest megyei szarvasmarhatelepen használt 5 különböző ivarzásindukáló gyógyszer (Alfaglandin, PGF, Dinolytic, Gonavet, Ovarelin) és ezen belül 3 hatóanyag (D-Phe6-gonadorelin, kloprosztenol és dinoproszt-trometamin) sorsát követtük nyomon a felhasználástól egészen a hígtrágyában való megjelenéséig, 2017-től 2020-ig. A tanulmány során áttekintettük a gyógyszerfogyást, valamint minden évben negyedéves ciklusokban, évszakonként vizsgáltuk meg a telepen keletkezett hígtrágya hormonhatását. Külön teszteltük a telepen alkalmazott hormonkészítmények hormonhatását is. Az ösztrogénhatás vizsgálatokhoz a humán ösztrogénreceptort tartalmazó élesztőtesztet alkalmaztuk az ISO 19040 szabvány alapján. Az eredmények statisztikai értékelésével (Pearson-féle korreláció és főkomponens-elemzés) az ivarzásindukálók felhasználása, a telep szaporodásbiológiája és a hígtrágya ösztrogénhatása közötti összefüggéseket tártuk fel. Megállapítottuk, hogy a hígtrágya és az iszap ösztrogénhatása erősen összefügg. Mindhárom vizsgált gyógyszerhatóanyag erős korrelációt mutatott a hígtrágya/iszap ösztrogénhatásával. Vizsgálataink alátámasztják, hogy a hígtrágya egy olyan anyag, melyet a szántóföldre történő kijuttatás előtt számos egyéb ok mellett a hormon- és gyógyszertartalma miatt is új kezelési módszerekkel kell ártalmatlanítani, nemcsak környezetegészségügyi szempontból, hanem az egészségügyi kockázatok miatt is, valamint hogy a megfelelő gyógyszerválasztással a hígtrágya hormonhatása redukálható.
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.
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.
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-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.
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.
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.
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.
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.
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.
Greenhouse plastic contaminations in agricultural soils were studied to quantify and examine the macroplastic and microplastic contaminants on the soil surface, soil profile, and groundwater under greenhouse farmland. Random sampling was used to select three areas in a greenhouse farm where macroplastic and microplastic data were collected. Four composite samples were collected from shallow (0–20 cm) and deep (20–40 cm) soils for each sampling point, respectively. Three soil profiles were dug, and samples were collected at intervals of 20 cm. Groundwater samples were also collected from the same profiles at a depth of 100 cm. Microplastics were extracted using predigestion of organic matter with 30% H2O2 and density separation with ZnCl2. The total mass of macroplastics in the greenhouse farmland was 6.4 kg ha–1. Polyethylene and polyvinyl chloride were the dominant plastic structures, and the dominant sizes were 1–5 and 0.5–1.0 cm, respectively. Overall, the average abundance of microplastics in the greenhouse soil was 225 ± 61.69 pieces/kg, and the dominant size structure was 2–3 mm. The average microplastic concentrations at depths of 0–20 and 20–40 cm were 300 ± 93 and 150.0 ± 76.3 pieces/kg, respectively. The average microplastic concentration in the groundwater was 2.3 pieces/l, and fibers were the dominant plastic structure. Given that microplastics were found in greenhouse soil, soil profiles, and groundwater, we recommend the careful cleaning and disposal of plastics on greenhouse farmland and further research to shed light on the level of microplastic contamination in the soil profiles and groundwater.
Abstract
A precise, sensitive, specific and accurate stability indicating densitometric method was developed and validated for alpha-lipoic acid (ALA) in bulk and capsule dosage form. The study employed pre-coated silica gel 60F254 TLC plates as stationary phase and toluene: chloroform: methanol: formic acid (5:3:1:0.05; v/v/v/v) as mobile phase. The developed method furnished compact spots of alpha-lipoic acid (Rf 0.28 ± 0.05) after derivatization, offered good linearity in range 80–400 ng/spot with correlation coefficient of 0.998. The values for detection and quantitation were found 18.022 and 54.612 ng/spot respectively. ALA was subjected to stress degradation studies and total 13 degradation products were resolved. Thus, the proposed method offered good results according to ICH guidelines, and can be used for identification, routine quantitative determination as well as for monitoring the stability of ALA in bulk and in capsules.
Abstract
Modafinil has a strong and long-lasting awakening effect. Short-term use can improve cognitive and work efficiency. Therefore, it has been known to be abused by students and parents as a “smart drug.” It is in the first category of psychotropic drugs and strictly controlled. To detect modafinil in rat plasma and study the differences in the pharmacokinetics of modafinil between oral and sublingual administration in rats, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed. Rats were injected with modafinil by oral gavage and sublingual vein, respectively, blood was collected within a certain period, and the plasma was obtained by centrifugation. Midazolam was used as the internal standard, and the concentration of modafinil in the plasma was determined by UPLC-MS/MS, where a drug-time curve was created to calculate the pharmacokinetic parameters. The standard curve for modafinil ranged from 1 to 2000 ng mL−1 with good linearity. The intra-day accuracy of modafinil was between 86% and 104%, and the intra-day accuracy was between 90% and 103%. Intra-day precision (RSD%) was less than 15%, inter-day precision (RSD%) was less than 15%. The matrix effect was between 93% and 102%, and the recovery was greater than 91%. The UPLC-MS/MS method established in this work has good selectivity and high sensitivity, and the UPLC-MS/MS method was successfully applied to the pharmacokinetics of modafinil by oral gavage and sublingual injection in rats. The bioavailability of modafinil was calculated to be 55.8%.
Abstract
A UPLC-MS/MS method was developed to determinate curdione in the mouse blood, and the pharmacokinetics of curdione in mice after intravenous (5 mg kg−1) and oral (20 mg kg−1) administration were studied. The HSS T3 column was used for separation, and column temperature was set at 40 °C. Multiple reaction monitoring (MRM) mode were used for determination of curdione. Blood samples were taken from the caudal vein of Institute of Cancer Research (ICR) mice after administration of curdione. It showed a good linear relationship in the range of 1–500 ng mL−1 (r > 0.998); the intra-day precision was <13%, the inter-day precision was <15%, and the accuracy was 90%–105%, the recovery was >77%, and the matrix effect was 97%–107%. The half-life was relatively short, and the bioavailability was 6.5%. The developed method was suitable for the pharmacokinetics of curdione in mice.
Abstract
A rapid and simple ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for simultaneous determination of six analytes from the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves (ESL) in beagle dog plasma for the first time, including 3-O-α-l-rhamnopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranosyl-30-norlean-12,20 (29) –dien-28-olic acid, ciwujianoside E, guaianin N, and eleutheroside K. The chromatographic separation was performed using an ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) using a gradient elution way with a mobile phase of acetonitrile-water containing 0.1% formic acid. Analytes were detected on a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source with multiple reaction monitoring (MRM) mode. Calibration curves were all linear (r ≥ 0.9933) over the concentration range. The mean extraction recoveries and matrix effect of analytes and I.S. were ranged from 80.26% to 98.32% and from 91.27% to 111.67%, respectively. The intra-day and inter-day precision were ranged from 2.20% to 14.81%, and the accuracy range was 1.60–14.60%. The analytical method was successfully applied for the pharmacokinetic characteristics of the six analytes in beagle plasma after oral administration of ESL extracts. The T 1/2 of six analytes was more than 3.09 ± 0.78 h.
Abstract
Epilepsy is one of the most prevalent neurological conditions and antiepileptic drugs are the mainstay of epilepsy treatment. High variation in pharmacokinetic profiles of several antiepileptic drugs highlights the importance of therapeutic drug monitoring to estimate pharmacokinetic properties and consequently individualize drug posology. In this work, a simple, rapid and robust liquid chromatography-tandem mass spectrometry method was developed for simultaneous quantification of carbamazepine and its metabolite carbamazepine-10,11-epoxide, gabapentin, levetiracetam, lamotrigine, oxcarbazepine and its metabolite mono-hydroxy-derivative metabolite, phenytoin, topiramate, and valproic acid in human plasma for therapeutic drug monitoring. d 6 -Levetiracetam, d 4 -gabapentin and d 6 -valproic acid were used as internal standards. After addition of internal standards along with two-step protein precipitation and dilution sample preparation, plasma samples were analyzed on a C18 column using a gradient elution in 5 min without interference. The calibration curves were linear over a 100-fold concentration range, with determination coefficients (r 2 ) greater than 0.99 for all analytes. The limit of quantification was 0.5 μg mL−1 (0.1 μg mL−1 for oxcarbazepine, 2 μg mL−1 for levetiracetam, and 10 μg mL−1 for valproic acid) with precision and accuracy ranging from 3% to 9% and from 94% to 112%, respectively. Intra- and inter-day precision and accuracy values were within 15% at low, medium and high quality control levels. No significant matrix effect was observed in the normal, hemolyzed, lipemic, and hyperbilirubin blood samples. This method was successfully used in the identification and quantitation of antiepileptic drugs in patients undergoing mono- or polytherapy for epilepsy.
Abstract
A rapid, selective, and precise high performance thin layer chromatographic method was developed and validated for the simultaneous analysis of paracetamol, caffeine, phenylephrine and chlorpheniramine in tablets. The chromatographic analysis was carried out on glass plates pre-coated with silica gel 60 F254 as a stationary phase. The optimized mobile phase was methanol : n-butanol : toluene : acetic acid (8:6:4:0.2 v/v). TLC chamber of 10 × 20 cm was used with saturation time of 15 min. The retardation factor (RF) for chlorpheniramine, phenylephrine, caffeine and paracetamol was found to be 0.15 ± 0.02, 0.29 ± 0.02, 0.50 ± 0.02, 0.68 ± 0.02 respectively. Detection was carried out at 212 nm. Validation study was done following ICH Q2 (R1) guideline. The regression data for the calibration plots showed good linear relationship with R 2 = 0.997 over the concentration range of 300–1,500 ng band−1 for caffeine, R 2 = 0.996 over the concentration range of 100–500 ng band−1 for phenylephrine, R 2 = 0.996 over the concentration range of 200–600 ng band−1 for chlorpheniramine, R 2 = 0.998 over the concentration range of 400–2,400 ng band−1 for paracetamol. The method was validated for precision, accuracy and recovery. Minimum detectable amounts were found to be 304.9 ng band−1, 87.88 ng band−1, 117.18 ng band−1 and 143.06 ng band−1 for caffeine, phenylephrine, chlorpheniramine, and paracetamol respectively while the limit of quantification was found to be 923.95 ng band−1, 266.32 ng band−1, 355.11 ng band−1, and 433.53 ng band−1 in the same order. The method was successfully applied to analyze two marketed tablets in a selective and reproducible manner.
Egy köles tájfajta műtrágya-reakciójának vizsgálata
Examination of the reaction to fertilization of regional millet variety
Kutatómunkák általános célja olyan kísérletek végzése, amelyek feltárják az adott régióban perspektivikusan termeszthető fajták, illetve tájfajták optimális műtrágyázási igényeit. Tanulmányunkban a Karcagon nemesített és fenntartott ’Maxi’ köles tájfajta tápanyagreakciójának vizsgálatából származó eredményeinket mutatjuk be a módosított Országos Műtrágyázási Tartamkísérlet (OMTK) 2017. évi és az annak figyelembevételével 2021-ben beállított Műtrágyázási Kísérleti Kert (MKK) adatai alapján. A kísérleteket Karcagon, a MATE Karcagi Kutatóintézetben, egy mélyben szolonyeces réti csernozjom talajon állítottuk be. 2017-ben a módosított OMTK kezelései 4 nitrogén (40, 80, 120, 160 kg ha– 1), 4 foszfor (0, 40, 80, 100 kg ha– 1) és 3 kálium (0, 60, 90 kg ha– 1) dózis kombinációjából adódtak, illetve volt egy műtrágyázás nélküli abszolút kontroll. 2021-ben az MKK kezelései 3 nitrogén (40, 80, 120 kg ha– 1), 3 foszfor (0, 40, 80 kg ha– 1) és 2 kálium (0, 60 kg ha– 1) dózis kombinációját foglalták magukba, illetve mindegyik parcella felére növénykondicionáló szert juttatunk ki. A termesztett növény mindkét évben a karcagi nemesítésű ’Maxi’ kölesfajta volt. A különböző kezeléscsoportok termésre gyakorolt hatásának statisztikai értékelését egytényezős varianciaanalízissel végeztük el. Mindkét vizsgálati évben a 80 kg ha– 1 hatóanyag mennyiségben kijuttatott nitrogén műtrágyázás bizonyult a leginkább megfelelőnek. A magas foszfor dózisok a legtöbb esetben termésdepresszióhoz vezettek. Eredményeink alapján még a közepes – jó kálium ellátottságú karcagi talajokon is hasznos lehet a kálium kijuttatása, bár a káliumtrágyázás termésre gyakorolt hatását a varianciaanalízis nem igazolta. Az Algomel PUSH szerrel végzett növénykondicionálás statisztikailag is igazolhatóan, mintegy 10%-kal növelte a termés nagyságát. Kutatómunkánk folytatásával pontosabban meghatározható lesz számos tájfajta tápanyagreakciója és fajtaspecifikus, a helyi agroökológiai viszonyokat is figyelembe vevő tápanyag dózisok és kombinációk ajánlhatók a gazdálkodóknak.
The general objective of our research is to carry out experiments that are suitable to reveal the optimal fertilization demand of regionally bred or potentially producible crop varieties for a specific region. In our recent study, the results gained from the examination of the nutrient reaction of the regional millet variety ‘Maxi’ bred and maintained in Karcag are introduced based on the data originating from the modified Long-term National Fertilization Experiments (OMTK) in 2017 and from the Fertilization Experimental Garden (MKK) established at Karcag in 2021. Both experiments were set up in the MATE Research Institute of Karcag on a meadow chernozem soil salty in the deeper layers. In 2017, there were 4 nitrogen (40, 80, 120, 160 kg ha−1), 4 phosphorus (0, 40, 80, 100 kg ha−1), and 3 potassium (0, 60, 90 kg ha−1) dosage combinations applied and one unfertilized absolute control in the OMTK trial. In 2021, in the MKK experiment, treatments involved 3 nitrogen (40, 80, 120 kg ha−1), 3 phosphorus (0, 40, 80 kg ha−1), and 2 potassium (0, 60 kg ha−1) dosage combinations, furthermore, on half of the plots a plant conditioner was sprayed. Millet variety ‘Maxi’ bred at Karcag was the indicator crop in both years. For the statistical analysis of the effect of the various treatment groups on yields, One-way ANOVA tests were used. We considered the 80 kg ha−1 nitrogen substance dose the most suitable in both years. High dosage of phosphorus application resulted in yield depression in most of the cases. Based on our results, potassium fertilization can be effective even on the soils of Karcag with medium to good potassium supplies, though the analysis of variance did not justify the effect of K-fertilization on yields. The 10% yields increase due to plant conditioning with Algomel PUSH was statistically proven. By continuing or research, the reaction to fertilization of several regional crop varieties can be determined more precisely, and variety-specific nutrient doses and combinations can be determined and suggested to the local famers taking the regional agri-ecological conditions into consideration.
Abstract
Perampanel (PER) is the first clinically available selective antagonist of α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA) receptor approved globally for the treatment of epilepsy. Studies have recently underlined the significant association between dose-exposure-effect-adverse events of PER in patients with epilepsy, so the therapeutic drug monitoring (TDM) of PER is critical in clinical practices, especially for pediatric patients with drug-resistant epilepsy. Due to several limits in previous published analytical methods, herein, we describe the development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for monitoring PER in human plasma samples. Protein precipitation method by acetonitrile containing PER-d5 as internal standard was applied for the sample clean-up. Formic acid (FA, 0.2 mM) in both aqueous water and acetonitrile were used as the mobile phases and the analyte was separated by an isocratic elution. Qualification and quantification were performed under positive electrospray ionization (ESI) mode using the m/z 350.3 → 219.1 and 355.3 → 220.0 ions pairs transitions for PER and PER-d5, respectively. Potential co-medicated anti-seizure medications (ASMs) have no interference to the analysis. Calibration curves were linear in the concentration range of 1.00–2,000 ng mL−1 for PER. The intra- and inter-batch precision, accuracy, recovery, dilution integrity, and stability of the method were all within the acceptable criteria and no matrix effect or carryover was found. This method was then successfully implemented on the TDM of PER in Chinese children with drug-resistant epilepsy. We firstly confirmed the apparent inter- and intra-individual PER concentration variabilities and potential drug-drug interactions between PER and several concomitant ASMs occurred in Chinese pediatric patients, which were also in line with previous studies in patients of other race.
Abstract
Gluten-free (GF) breads are often described with low quality, rapidly staling, dry mouthfeel and crumbling texture attributes. In lack of recent texture profile data on commercially available, preservative-free, freshly-baked GF bread, this study aimed to compare different types of GF products with their wheat-based counterparts during a 4-day-long storage test. Texture analysis data showed that GF loaves performed better than or comparable to the wheat-based ones in hardness, springiness and cohesiveness. Among sensorial properties mouth-feel, softness and aroma were evaluated as significantly better or similar for GF versus wheat-based products. GF cob had a saltier taste, which reduced the flavour experience. Both the texture results of the storage test and sensory data showed that the quality of GF bread products improved in recent years; they stayed comparable with their wheat-based counterparts even during a 4-day-long storage period.
The selectivity of the separation of five antihistamines has been investigated by TLC on silica gel 60 F254 and on aluminium oxide 60 F254 with a variety of mobile phases in horizontal chambers. The best separation selectivity and retention differences for the drugs on the two types of plate were obtained with the mobile phases chloroform–ethyl acetate, 1 + 1 (v/v), ethyl acetate, and butan-2-one–toluene, 7 + 3 (v/v).
The plates were visualized by illumination at l = 254 nm and by reaction with different reagents. The greatest detection sensitivity – 0.06 mg for cetirizine, 0.1 mg for chloropyramine, and 0.2 mg for antazoline, doxylamine, and ketotifene – was obtained by spraying with potassium iodoplatinate reagent.
Knowledge of the composition of an incorporated alloy is a precondition for avoiding polymetallism in subsequent prosthetic treatment, or detection of the cause of an allergic reaction attributed to a metallic component of the prosthesis restoration. The method proposed in this paper can be a very useful means of determining the presence of Ni–Cr or Co–Cr dental alloys, and, especially, beryllium in Ni–Cr alloys which, despite its toxicity, gives the alloy desirable properties. Nickel is also a well-known allergen. This paper reports an analytical procedure for detection and identification of cobalt-and nickel-based dental alloy components. The method involves anodic sampling, and separation and identification of the components by thin-layer chromatography on precoated microcrystalline cellulose layers. Computer-assisted optimization was used to choose the mobile-phase composition. Excellent detection and identification of nickel, chromium, cobalt, molybdenum, and beryllium, on the basis of different RF values and spot colors, was achieved after anodic sampling in-situ.
Microanodic dissolution of dental alloys enables intra-oral, in-situ, and almost non-destructive sampling of a permanent prosthesis restoration.
The object of this study was determination of the content and composition of the essential oil of the fruits of three varieties of stalk celery – Helios, Zefir, and Orient. We also investigated hexane extracts obtained from the fruits of two varieties of stalk celery – Helios and Zefir. The essential oils and the extracts were examined by TLC and GC–MS.
Analysis showed the presence of terpene (mono- and sesquiterpene) and non-terpene (phthalide) fractions in the oils and extracts investigated. The combined amount of limonene, α- and β-pinene and myrcene in the monoterpene fraction of the essential oils ranged from 79.1 to 82.9%. The amount of the sesquiterpene fraction (α-and β-selinene) was from 15.7% to 18.8%. The phthalide fraction (3-n-butylphthalide, dehydrosedanolide, and sedanolide) was found in trace amounts. The amounts of these fractions in the hexane extracts ranged from 40.2 to 43.6% for the monoterpene fraction, from 19.4 to 20.7% for the sesquiterpene fraction, and from 35.7 to 37.7% for the phthalide fraction.
The conditions used for TLC and HPTLC analysis of catechins have been optimized. Chemically modified stationary phases (HPTLC CN, HPTLC NH2, and HPTLC RP-18W) were used for qualitative examination of polyphenol fractions obtained by an SPE–RP 18 method from Uncaria tomentosa bark. Although the best separation of catechin from epicatechin was achieved on octadecyl plates, silica gel plates are good enough for preliminary investigations of crude plant extracts.
A high performance thin layer chromatographic method has been developed for the determination of idebenone in pharmaceutical preparations. The method uses silica gel 60 F254 as the stationary phase, toluene–diethyl ether–methanol–triethylamine, 4 + 4 + 1.5 + 0.5 (v/v) as mobile phase, and detection at λ = 279 nm, the wavelength of maximum absorption of idebenone. Diclofenac sodium was used as internal standard. The response was found to be linearly dependent on amount of idebenone between 100 and 1000 ng mL–1. The method was validated to determine its accuracy and precision and the repeatability of the method was also determined. System suitability tests were conducted to verify that the resolution and reproducibility of the chromatographic system are adequate for the analysis. The determination of idebenone in tablets is described.
A quantitative instrumental high-performance thin-layer chromatographic (HPTLC) method has been developed for assessment of the photodegradation of bensulfuron-methyl on silica gel. The method uses automated band application on to silica gel plates with fluorescent indicator, direct development after irradiation, and scanning densitometry of fluorescence-quenched zones of samples and standards. The accuracy of the analyses was confirmed by performing recovery studies with preanalyzed samples and a blank sample fortified with the analytes. Precision was determined by analyzing samples in replicate; loaded amounts of 500–2000 ng per spot were suggested for assessing the photodegradation of the pesticides. The simplicity of sample preparation and the chromatographic techniques, high sample throughput, high reproducibility, and the strong possibility of separating the photoproducts seem to make the test on HPTLC plates highly suitable for estimation of the photodegradability of pesticides in the adsorbed state.
Homologous series of higher fatty acids, higher alcohols, and methyl esters of higher fatty acids have been separated by RPTLC. The values of R M and of the log P Rek partition coefficient from Rekker for the compounds of the homologous series could be correlated with numerical values of topological indexes based on the adjacency matrix (M, °χ, 1χ, °χν, 1χν ), and on the distance matrix (W, A, °B,1B). The most accurate prediction of the R M and log P Rek values of the compounds investigated was achieved by use of monoparametric equations containing one topological index based on the adjacency matrix.
Two-dimensional thin layer chromatography of twelve flavonoids and three phenolic acids from Betula sp. leaves has been performed in normal-phase systems. Plots showing the dependence of RM on modifier concentration in some non-aqueous systems were used to optimize the chromatographic separation. RM values were correlated for all the chromatographic systems investigated and optimum pairs of systems were then selected for use in two-dimensional TLC separations. Complete separation of the compounds investigated was achieved by use of two optimum non-aqueous mobile phases on silica plates.
The normal-phase (NP) and reversed-phase (RP) thin-layer chromatographic separations of aminoglycosides (streptomycin, kanamycin, gentamycin, and tobramycin) have been investigated on silica gel and C18 plates, respectively. The mobile phase acetone–2% sodium acetate–acetic acid–butanol, 7 + 6 + 4 + 1 (v/v) was successful for NPTLC and acetonitrile–5 mM sodium acetate buffer (pH 4.6) 4 + 18 (v/v) for RPTLC. The spots were located by use of iodine vapor. The minimum detection limits were in the range 0.4–0.6 μg. The method is a simple and direct approach for detection which does not require pre- or post-chromatographic derivatization.
Complexes of hydroxy- and alkyloxytetraphenylporphyrins with Cu (II), Zn (II), and Ni (II) have been prepared and their chromatographic behavior in adsorption and partition thin-layer chromatography has been investigated. Gutman topological indexes, Mν, and the screening effect, SE, of the hydrocarbon chains on the electron pairs of the oxygen atoms of –OR groups have been calculated for the metalloporphyrin derivatives studied. The correlation between these and chromatographic retention, expressed as RM values, has been studied.
Planar electrochromatography (PEC) is a mode of planar chromatography in which the mobile phase is driven by electroosmotic flow. The variables that affect the performance of PEC with an aqueous mobile phase on a bonded octadecylsilyl layer are discussed. These include the magnitude of the applied electric field, the concentration of the buffer salt, the pH of the mobile phase, and the concentration of acetonitrile used as the organic modifier. The effect of changing each of these variables is illustrated by model separations of a mixture of four compounds of diverse structure.
Planar chromatographic methods thin-layer chromatography (TLC) and over-pressure thin-layer chromatography (OPLC) have been developed for the determination of pigments in plant leaves. Plants with variegated leaves, which sometimes contain both anthocyanins and chlorophyll, are a reasonable material for investigation. Multicolored Coleus, Prunus cerasifera, and Rhus hirta leaves were taken for quantitative determination of anthocyanins and chlorophyll. The separation of pigments from plant leaves, which depends on compound polarity was optimized by appropriate selection of mobile and stationary phases and chromatographic conditions.
The chromatographic behavior of fullerene C60 has been studied on silica gel layers impregnated with solutions of glucose, sucrose, fructose, and dextrans of MW 20, 40, and 110 kDa, and with hexane as mobile phase. It was found that the RF of fullerene decreases as the concentration of impregnating solution is increased. The retention of fullerene C60 changes to a smaller extent when dextran solutions are used.
The solid-phase interaction of fullerene with the carbohydrates sucrose and dextran was studied by use of differential scanning calorimetry (DSC) and by NMR and UV-vis spectroscopy. The interaction with sucrose is greater than that with the dextrans.
Correlation was observed between the chromatographic behavior of C60 fullerene and the solid-phase interaction of the compound with carbohydrates.
Carbohydrates have been examined by TLC on layers modified with metal ions, in the form of salts, by dipping commercial plates in methanolic solutions or by use of mobile phase additives; the mobile phases were mixtures of acetonitrile, propan-2-ol, or acetone with water or aqueous solutions of the metal salts. The effect on spot shape and retention of the identities and concentrations of the metal ions used for impregnation are discussed, and the selectivity of the different systems investigated are compared. The chromatographic properties of the adsorbents used were compared by consideration of the relationships between RM values measured on the different layers.
In normal TLC practice, migration of the mobile phase through the layer is controlled by capillary forces. Under these conditions the velocity at which the solvent front moves is a function of the distance of the front from the solvent entry position, and this velocity declines as the distance increases. In this work we have proved that the velocity and migration distance of the mobile-phase front in porous media can be increased by application of an external electric field. We have called this displacement effect on liquids ‘dielectroosmotic flow’ (DEOF), because of its similarity with electrokinetic phenomena. Capillary tubes were used to enable understanding of the flow phenomena which occur in porous media.
A stand-alone argentation TLC (Ag-TLC) procedure has been established for rapid estimation of the authenticity and densitometric quantitation of fatty acid groups in milk fats. The applicability of methyl (ME) and isopropyl (IPE) ester derivatives for accurate short-chain fatty acid analysis by Ag-TLC and GLC was compared and a correction coefficient compensating for loss of C4–C10 saturated fatty acids has been proposed. To check its accuracy and reproducibility the method was applied to model mixtures and to real margarine and butter samples. Low levels of trans fatty acids can be unequivocally detected and amounts down to 0.2% can be measured precisely. The method gives a good estimate of the diversity of isomeric fatty acids in the samples and when precautions are taken to avoid overloading, it provides reliable results with good accuracy.
A simple and reliable HPTLC method has been developed and validated for the determination of dexamethasone (as the sodium phosphate salt) and xylometazoline (as the chloride). Assay of the compounds was performed on silica gel HPTLC plates with spherical particles by development with the mobile phase ethyl acetate–acetonitrile–diethylamine–water, 3 + 3 + 1 + 1 (v/v). A TLC scanner set at λ = 240 nm was used for direct evaluation of chromatograms in reflectance/absorbance mode. The validation data linearity (R > 0.996), precision (RSD = 1.67–2.77%), accuracy (recovery = 95.95–100.69%) and LOD and LOQ (ng levels) were determined and found to be satisfactory.
Assay of dexamethasone and xylometazoline in nasal drops was performed simultaneously with assay of preservatives such as methyl para-hydroxybenzoate. The effect of the most commonly used preservative, benzalkonium chloride on the concentrations of active substances was investigated; it was found that this compound led to a significant reduction of the dexamethasone sodium phosphate content of nasal drops.
A method developed for quantitative determination of the total amount of polyaromatic hydrocarbons (PAH) in human hair has been applied to the analysis of smokers’ hair. The procedure involves washing the hair with dichloromethane, acid decomposition of the hair matrix, micro-liquid extraction, and HPTLC determination of total PAH concentrations in the whole extract. The concentrations of PAH in human hair were in the range 0.005–0.3 μg g–1 hair.
High-performance thin-layer chromatography (HPTLC) on silica plates, with two successive mobile phases, has been used for analysis of seven amine azo dye isomers prohibited under a German ban. Dichloromethane was used for the first development, to a distance of 4.5 cm. After drying, the second development was performed with toluene–tetrahydrofuran, 10 + 1 (v/v), to a distance of 8.5 cm. Spots were visualized at λ = 254 nm. Eighteen amines have been studied by use of the method. The limit of determination (X) and the correlation coefficient in the range X to 5X are reported for each amine. To increase the sensitivity of detection, the UV spectrum was acquired for each amine and the wavelength of maximum absorbance (λmax) was used to establish the limit of determination. Synthetic mixtures and dye samples have been resolved and quantified.
This paper reports a recently developed technique, coupling of optimum-performance laminar chromatography (OPLC) with online radioactivity detection (OPLC–RD). Sample preparation for purification of urinary metabolites of a 14C-labeled drug candidate was performed on octadecyl-modified silica solid-phase extraction columns. Optimum-performance laminar chromatography was conducted on aluminum-backed silica gel layers with butanol– acetic acid–water as mobile phase. Eluate radioactivity was detected by use of a flow-cell radioactivity detector equipped with solid scintillator, and eluate fractions containing radioactivity were collected. Strongly retained radioactive components were detected off-line after development by use of digital autoradiography (DAR).
The isolated fractions containing metabolites were further purified by reversed-phase high-performance liquid chromatography coupled with radioactivity detection; this provided a second dimension for additional selectivity. Purified metabolite fractions were submitted to structure elucidation by spectroscopic methods.
The novel on-line optimum-performance layer chromatography with radioactivity detection, combined with high-performance liquid chromatography with radioactivity detection and digital autoradiography techniques, the advantages and disadvantages of which are discussed in detail in this paper, provides a rapid, effective, and economic tool which can be applied to advantage in metabolism research.
In this paper we report our most recent experimental results relating to the thermal instability of selected alkyl chemically bonded stationary phases. The phenomenon of the thermal instability of such phases, as a result of their irradiation with a high-power neodymium laser, the light source of a Raman spectrometer, has been demonstrated in a series of our earlier publications. We even established a novel method of estimating the density of coverage of the silica matrix with alkyl ligands by utilizing the thermal instability of the phases discussed. The mechanism of the thermal transformation of alkyl chemically bonded ligands remained rather obscure, however, vague speculations only were made about the possible aromatization of these ligands.
In this paper we provide additional experimental evidence in support of our earlier hypothesis about possible aromatization of alkyl ligands on the surface of the acidic/basic silica matrix under the influence of high temperature. This evidence was obtained by use of instrumental techniques such as Raman spectroscopy, differential scanning calorimetry (DSC), and UV absorption spectroscopy. Although all these techniques supply indirect evidence only, the results reported furnish a convincing confirmation of our earlier intuitions.
The effect of cold-stress (2°C, 7 days cold-hardening) on the level of polyamines in different varieties of wheat and genetically modified wheat samples (chromosome substitution lines, deletion lines, recombinant lines) has been investigated. Biogenic amines (spermine, spermidine, putrescine, and agmatine) were determined as the dansyl derivatives by stepwise gradient elution with the Personal OPLC BS 50 Chromatograph. Short-term cold-hardening caused characteristic changes in free polyamine content of wheat genotypes. The total free polyamine content was significantly lower in the cold-hardened samples than in the control samples. It seems that accumulation of spermine and agmatine might be good markers of cold sensitivity.
A quantitative thin layer chromatographic (TLC) method on silica gel, with ethyl acetate–acetone–alcohol, 62 + 40 + 3 (v/v) as mobile phase, has been developed for the determination of olaquindox at ppm levels in animal feed. Preliminary purification consists of extraction with water, adsorption on XAD-4, washing, and elution with acetonitrile. Before the elution step acetylolaquindox is added as internal standard. The residue obtained after evaporation of acetonitrile is dissolved in a small volume of methanol. Quantitation is performed by densitometry at λ = 360 nm.
Abstract
A modified QuEChERS method using a GC-ECD to determine the multiple residues of pyraclostrobin, difenoconazole, dimethomorph and azoxystrobin and to indirectly determine the total residues of maneb, mancozeb and propineb by a GC-FPD (with an S filter) was established and validated. Meanwhile, field trials were conducted in accordance with good agricultural practice (GAP) to study their characteristics of residue degradation under the agricultural climate and cropping system of Guangxi Province. The separation effect of each target peak was good with a linearity range of 0.01–5 mg L−1, a limit of detection (LOD) of 0.003–0.015 mg kg−1 and a limit of quantification (LOQ) of 0.01–0.05 mg kg−1. The average recovery ranges of vegetable tomatoes and cherry tomatoes were 70.5–120.0% and 70.8–119.8%, respectively, with relative standard deviations (RSDs) of less than 7.1%. Field trials of seven fungicides in vegetable and cherry tomatoes showed that the half-lives (t 1/2 ) of the dithiocarbamate fungicides (metiram, mancozeb, and propineb, defined as total residues determined as CS2), pyraclostrobin, difenoconazole, dimethomorph, and azoxystrobin were in the ranges of 5.2, 12.7–17.8, 7.6–7.9, 6.6–6.9, and 6.3–6.6 d in vegetable tomatoes, respectively. The cherry tomatoes presented ranges of 4.3–4.5, 10.8–11.8, 6.7–7.0, 5.4–5.5, and 5.9–6.2 d, respectively. Combined with the final residue and market monitoring results, the results show that cherry tomatoes have significantly higher terminal residues, initial deposits, and maximum residues of seven fungicides than vegetable tomatoes, and these seven pesticides can be detected in cherry tomatoes purchased from three markets. Therefore, cherry tomatoes may be regarded as representative varieties of tomatoes in realizing residual extrapolation for the establishment of the maximum residue limit (MRL) value of fungicides in tomatoes and for conducting market monitoring.
The chromatographic behavior of six macrocyclic antibiotics (erythromycin, troleandomycin, tylosin, vancomycin, rifamycin B, and rifampicin) has been examined on Polyamide 11F254 TLC plates as stationary phase with five binary solvent mixtures (methanol–water, ethanol–water, propanol–water, acetonitrile–water, and tetrahydrofuran–water) as mobile phases in which the concentration of the organic modifier was from 0 to 100% (v/v). Chromatographic retention data and a possible retention mechanism are discussed.
