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Abstract

A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.

Open access

Abstract

In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with both detection techniques such as diode-array detection and fluorescence detection (HPLC-DAD-FLD) for the determination of nesfatin-1 in fetal bovine serum samples. The limit of detection (LOD) and limit of quantification (LOQ) for nesfatin-1 were set at satisfactory values in the range 0.22–0.35 mg mL−1 and in the range 0.67–1.05 mg mL−1, respectively (at two different wavelengths (DAD) and at four different wavelengths (FLD)). Analyte concentrations were determined as the average value from fetal bovine serum matrix samples. The preliminary results show that the SPE procedure on Isolute Si-TsOH (SCX-3) could be used for further nesfatin-1 analyses in human serum samples. Both the SPE technique, chromatographic analysis with gradient elution mode and detection technique are fast and convenient.

Open access
Progress in Agricultural Engineering Sciences
Authors:
N. Anter
,
M. Y. Guida
,
M. Kasbaji
,
A. Chennani
,
A. Medaghri-Alaoui
,
E. M. Rakib
, and
A. Hannioui

Abstract

In this scientific paper, thermochemical conversion of redwood (RW) was studied. Using the thermogravimetric analysis' technique (TGA), the thermal behavior of RW samples was examined at four heating rates ranging from 5 to 20 K min−1 in inert atmosphere between 300 and 900 K. Two main objectives have been set for this study; the first one was the determination of the kinetic decomposition parameters of RW (Pinus sylvestris L.), and the second one was the study of the variation of characteristic parameters from the TG-DTG curves of the main RW's components, such as; cellulose, hemicellulose and lignin. The kinetic analysis was performed using three isoconversional methods (Vyazovkin (VYA), Friedman (FR) and Flynn-Wall-Ozawa (FWO)), Avrami theory method and the Integral master-plots (Z(x)/Z(0.5)) method to estimate activation energy (E a ), reaction order (n), pre-exponential factor (A) and model kinetic (f(x)) for the thermal decomposition of cellulose, hemicellulose and lignin components.

The DTG and TG curves showed that three stages identify the thermal decomposition of RW, the first stage corresponds to the decomposition of hemicellulose and the second stage corresponds to the cellulose, while the third stage corresponds to the lignin's decomposition. For the range of conversion degree (x) investigated (0.1 ≤ x ≤ 0.7), the mean values of apparent activation energies for RW biomass were 127.60–130.65 KJ mol−1, 173.74–176.48 KJ mol−1 and 197.21–200.36 KJ mol−1 for hemicellulose, cellulose and lignin, respectively. Through varied temperatures from 550 to 600 K for hemicellulose, from 600 to 650 K for cellulose and from 750 to 800 K for lignin, the corresponding mean values of reaction order (n) were 0.200 for hemicellulose, 0.209 for cellulose and 0.047 for lignin. The pre-exponential factor's average values for three components of RW ranges from 0.08 × 1012 s−1 to 2.5 × 1012 s−1 (A hemicellulose = 1.09 × 1012 s−1), 0.10 × 1014 s−1 to 0.28 × 1014 s−1 (A cellulose = 0.17 × 1014 s−1) and 3.07 × 1016 s−1 to 3.69 × 1016 s−1 (A lignin = 3.33 × 1016 s−1), respectively. The experimental data of RW had overlapped the D 4, D 2 and F 3 in the conversion degree of 10–30%, 30–55% and 55–70% for the three components, respectively.

Open access

Abstract

A new method for the analysis of four target flavonoids in two kinds of citrus samples by ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed. Main variables affecting the UHPSFC separation were optimized, and under the optimized conditions the four target compounds (tangeretin, nobiletin, hesperetin and naringenin) can be separated within 10 min. The UHPSFC method allowed the determination of the four target compounds in the diluted stock solutions with limit of detection (LOD) ranging from 1.08 to 2.28 μg mL−1, and limit of quantification (LOQ) ranging from 1.45 to 4.52 μg mL−1, respectively. The coefficients of determination (R 2) of the calibration curves were higher than 0.9950. The recoveries of the four target compounds at three different concentrations were in the range of 82.4–117.6%. The validation results demonstrated that the proposed method is simple, accurate, time-saving and environment friendly, and it is applicable to a variety of complex samples such as medicine-food dual purpose herbs and functional foods.

Open access

Abstract

To overcome the problems of seasonality and geographical location in fruit production and processing, the production of aseptic semi-finished juice is an excellent solution. Even without refrigeration, aseptic pressing has a shelf life of more than a year, making it possible to produce finished products all year round. The production technology involves the addition of ascorbic acid to the pulp to fix or preserve colour. There is an increasing customer demand for ascorbic acid substitutes on the international market. In Hungary, one of the most important exports is aseptic sour cherry juice. In our work, ascorbic acid used for colour fixation was replaced by acerola concentrate. The anthocyanin content and colour coordinate values (L*, a*, b*, H, C) of aseptically filled sour cherry juice were determined and compared with the control sample during the 12 months of storage.

Open access

Abstract

Ziprasidone is the second generation antipsychotic drug with unique multipotent G-protein-coupled (GPCR) receptor binding profile. Since ziprasidone is a highly lipophilic and unstable compound, development of efficient method for a concurrent assay of ziprasidone and its main impurities was a very challenging task.

The UHPLC-MS/MS method that we developed for simultaneous determination of ziprasidone and its main impurities (BITP, Chloroethyl-chloroindolinone, Zip-oxide, Zip-dimer, and Zip-BIT) was compared with some other related HPLC-UV methods of our own and other authorship. An increase of the mobile phase pH value from 2.5 to 4.7 units in the examined analytical methods influenced elution order of the investigated compounds. It was found out that the UHPLC-MS/MS method is more selective and sensitive than the earlier developed HPLC-UV method. Similar to our earlier HPLC-UV method, the UHPLC-MS/MS method is linear with a correlation coefficient (r) above 0.99 for all the analysed compounds, but with a negligibly lower precision and accuracy. Finally, with shorter analysis time, smaller column size and reduction of solvent consumption, UHPLC-MS/MS is assumed as a greener method than HPLC-UV for the ziprasidone purity assay.

After transfer of the UHPLC-MS/MS method to the UHPLC-DAD system, suitability of the UHPLC-DAD method for routine control of ziprasidone and its main impurities is examined and confirmed based on the retained good selectivity, resolution and short analysis time.

Open access

As a means of assisting the selection of promising soil classification systems, a set of criteria were presented and tested. Inside the studied slightly saline plot World Reference Base (WRB) and Hungarian soil classification (HU) were compared at all four levels in terms of class separability, correlation to biomass, parsimony and homogeneity of classes. WRB surpassed HU in terms of the very important homogeneity of classes only, but HU performed better in terms of class separability, correlation to biomass and parsimony of classes. With many possible classification units WRB categorized the soil into a large number of classes, but 67% and 78% of them were single-profile classes at levels 3 and 4, respectively inside the ca 0.9 km2 area.

Open access

Abstract

Wild edible plants (WEPs) can be widely found in the world and defined as native species that grow naturally in their natural habitat. They have become part of the traditional food as human diet and used in folk medicine to treat diseases. They are very rich in terms of nutraceuticals. Melatonin is a natural hormone providing several benefits for human health. It has functions such as regulating growth and development and increasing tolerance to environmental stress factors in plants. It is stated that the serum melatonin level in humans increases after intake of foods containing melatonin. This study examined the presence of melatonin in wild grown cornelian cherry fruits by UFLC-FD and determined suitable extraction and chromatographic conditions. The optimum mobile phase, excitation/emission wavelength, and extraction solvent were determined as methanol: water: acetic acid, 275/345 nm, and methanol: water: HCl, respectively. Melatonin content in fruits ranged from 130.82 to 201.84 ng g−1 in fresh fruit.

Open access

Szarvasmarhatartó telepen alkalmazott ivarzásindukáló hormonok megjelenése a hígtrágyában

Appearance of on-farm bovine reproductive hormones in the resulting slurry

Agrokémia és Talajtan
Authors:
Eduárd Gubó
,
Tibor Molnár
,
Pál Szakál
,
Dóra Pordán-Háber
,
Ákos Bede-Fazekas
, and
Judit Plutzer

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.

Open access