A new and rapid hydrophilic interaction liquid chromatographic method has been developed for the quantitative analysis of amlodipine besylate and its specific impurities (D, E, and F). For development of this method, a systematic approach which includes Design of Experiments methodology was applied. For the method optimization, Box–Behnken design and specific way Derringer's desirability function were applied. They provided identification of the optimal chromatographic conditions on the basis of obtained mathematical models and graphical procedures (three D graphs). The optimal chromatographic conditions were the analytical column ZORBAX NH2 (250 × 4.6 mm, 5 µm particle size); mobile phase consisted of acetonitrile-water phase (50 mM ammonium acetate, pH adjusted to 4.0 with glacial acetic acid) (90.5:9.5 v/v); column temperature 30 °C, mobile phase flow rate 1 mL min−1, wavelength of detection 230 nm. As other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of amlodipine besylate and its impurities in any laboratory under different circumstances has been proven.
Authors:Lei Gao, Peng Wang, Zhongxiang Chen, Shizhan Tang, Song Wu, Gang Li, and Dongli Qin
Pharmaceuticals which are widely used in aquatic can easily migrate into the environment and aquatic animals, and can increase the risk of drug resistance and allergic symptoms if consumed by humans. In order to achieve high-throughput analysis of pharmaceuticals with different physical and chemical properties from complex matrices, we developed a new method for various types pharmaceuticals in fish and shrimp tissue. Series solid-phase extraction (s-SPE) with different adsorbents was selected for extracting and purifying analytes with different paddings. s-SPE were combined with ultra performance liquid chromatography triple quadruple tandem mass spectrometry (UPLC-MS/MS) for the detection of 30 pharmaceuticals antibiotics in fish samples. This method was stabilized and reliable to determinate the pharmaceuticals in fish and shrimp samples. As the method combined multiple Chinese national standards method, it could be easily treat the multi-pharmaceuticals from the fish and shrimp samples once time. It provided for both quantitative and qualitative methods and they could be applied to single- or multi-residue methods.
Authors:Ranim I. Moussad, Randa A. Abdel Salam, Ghada M. Hadad, Alaa EL Gindy, Ahmed I. Foudah, and Eman A. Abdel Hameed
In this study, a simple, fully validated and rapid reversed-phase HPLC with photodiode array detector method was developed for the simultaneous determination of 11 selected phenolic antioxidants over 33 min in personal care and food samples containing extracts of green apple, pomegranate (Ponica granatum) and argan oil (Argania spinosa). The method was performed using NUCLEODUR C18 column 5 µm particle size and 12.5 cm length. The HPLC mobile phase was prepared as follows, solution A: 1% aqueous acetic acid and solution B: Acetonitrile. The method was gradient at flow rate 1.0 mL/min with a simple mobile phase, minimal sample preparation, and diminished organic solvent usage (3% acetonitrile for almost 90% of the run time). The detection was carried out at 278 nm. The method presented good precision and accuracy with RSD% values ranged between 0.33 and 1.94% and wide linear range. The developed method was successfully applied on 67 personal care and food products present in Egyptian market and can be used for routine screening in laboratory for the regular quality control of the antioxidant content for products containing the mentioned extracts.
Authors:Zoltán Kovács, Juraj Števek, Miroslav Fikar, and Peter Czermak
The enzymatic conversion of sucrose to fructo-oligosaccharides (FOS) catalyzed by Pectinex Ultra SP-L, a commercial enzyme preparation from Aspergillus aculeatus, under free condition was studied. A mathematical analysis of the transfructosylation reactions was carried out to estimate the dynamic and steady-state performance of an enzyme membrane reactor (EMR) and to compare the continuous production scheme with the traditional batch process realized in stirred-tank reactor (STR). Kinetic parameters were identified simultaneously from a series of progress curves obtained from STR and EMR experimental runs. Model estimates appeared to fit well to experimental observations under the studied reaction conditions. Although conventional batch reactor outperforms EMR in terms of conversion, EMR compares favorably regarding productivity. The on-site industrial implementation of this technology might be attractive for food manufacturers aiming at utilizing a value-added sweetener mixture with prebiotic properties.
Authors:V. Parrag, Z. Gillay, Z. Kovács, A. Zitek, K. Böhm, B. Hinterstoisser, R. Krska, M. Sulyok, J. Felföldi, F. Firtha, and L. Baranyai
One of the most important food safety issues is the detection of mycotoxins, the ubiquitous, natural contaminants in cereals. Hyperspectral imaging (HSI) is a new method in food science, it can be used to predict non-destructively the changes in composition and distribution of compounds. That is why, in the last decade, the potential of HSI has been evaluated in many fields of food science, including mycotoxin research.
The aim of the recent study was to test the feasibility of HSI for the differentiation according to the toxin content of cornmeal samples inoculated with Fusarium graminearum, Fusarium verticillioides and Fusarium culmorum and samples with natural levels of mycotoxins. Samples were measured in the near infrared wavelength range of 900–1,700 nm and mean spectra of selected regions of interest of each image were pre-treated using Savitzky-Golay smoothing and standard normal variate (SNV) method. On the spectra, partial least squares discriminant analysis (PLS-DA) was carried out according to the level of contamination. Partial least squares regression (PLSR) method was used to predict deoxynivalenol (DON) content of samples and the cumulative toxin content: the sum of fumonisins (FB1, FB2) and DON content of samples. Based on the promising results of the study, HSI has the potential to be used as a preliminary testing method for mycotoxin content in feed materials.
Schizonepeta tenuifolia Briq. (ST) has been used as an aromatic exterior-releasing medicine in clinical practice for thousands of years in China. Previous researches have revealed both volatile oil (STVO) and aqueous extract (STAE) from ST showed significant pharmacological activities, such as anti-virus, anti-inflammation, anti-oxidation, and immunoregulation. However, the influence between each other was still unknown. The purpose of this study was to compare the pharmacokinetic profiles of three main flavonoids (luteoloside, apigetrin, and hesperidin) in STAE to illustrate the influence of STVO. A liquid chromatography-tandem mass spectrometry (HPLC-MS) method was established to quantitatively analyze the three absorbed ingredients in the plasma of healthy rats. Biological samples were analyzed on an Agilent Eclipse Plus C18 column (3.0 mm × 150 mm, 3.5 μm) with gradient mobile phase (containing 0.2% formic acid and acetonitrile) at a flow rate of 0.8 mL/min. All the analytes and quercitrin (IS) were investigated with an electrospray ionization source (ESI) using multiple-reaction monitoring (MRM) in negative ionization mode. In addition, this quantitative method showed good linearities (r ≥ 0.9995) and the lower limits of quantification were 0.590–1.19 ng/mL. The intra- and inter-day precisions ranged 3.47–10.45% and 4.29–11.28% for the three analytes. The mean extraction recoveries were in the range of 77.41–109.79% and the average matrix effects were within 83.41–112.67%. The validated method has been fully applied to compare the pharmacokinetic parameters of the three flavonoid glycosides in rat plasma after oral administration of STAE and STAE+STVO. In comparison of luteoloside, apigetrin, and hesperidin in STAE group, it was found that different degree of increasing existed for the time to reach the maximum concentration (Tmax), elimination half-life time (T1/2), the area under the concentration curves (AUC0→t and AUC0→∞) and the maximum concentrations (Cmax) in STAE+STVO group. As can be seen from above results, STVO could improve the absorption and bioavailability of the three analytes. These findings would provide some active and strong basis of safe clinical application for ST and further exploitation for STVO from the perspective of drug–drug interaction.
Authors:M.Y. Guida, S.E. Lanaya, F.E. Laghchioua, Z. Rbihi, and A. Hannioui
This study deals with fast pyrolysis of sawdust wood waste (SWW) at the range of temperature 300–700 °C in a stainless steel tubular reactor. The aim was to experimentally investigate how the temperature, the particle size, the nitrogen flow rate (N2) and the heating rate affect bio-oil, bio-char and gaseous products. These parameters were varied in the ranges of 5–20 °C/min, below 0.1–1.5 mm and 20–200 mL min−1, respectively. It was concluded that both the temperature and heating rate have a significant effect on both yield of bio-oil and bio-char resulting from pyrolysis of SWW. The liquid products obtained at various pyrolysis temperatures were subjected into column chromatography after removal of asphaltenes (hexane insoluble). Obtained bio-oils (maltenes or hexane soluble) were classified as aliphatic, aromatic and polar sub-fractions. The maximum of bio-oil yield of 39.5 wt% was obtained at a pyrolysis temperature of 500 °C, particle size between 0.5 and 1 mm, nitrogen flow rate (N2) of 100 mL min−1 and heating rate of 5 °C/min. Liquid product (bio-oil) obtained under the most suitable and optimal condition was characterized by elemental analysis, Nuclear magnetic resonance spectroscopy (1H NMR and 13C NMR), Fourier transformed infrared spectroscopy (FT-IR). The analysis of liquid showed that bio-oil from SWW could be a potential source of renewable fuel production and value added chemical. The yield of char generally decreases with increasing the temperature, the char yield passes from 54.61 to 29.47 wt% at the heating rate of 5 °C/min and from 50.01 to 24.5 wt% at the heating rate of 20 °C/min at the same range of temperature (300–700 °C). Solid products (bio-char) obtained in the presence of nitrogen (N2) contain a very important percentage of carbon and high heating values (HHVs).
Authors:Csihon Ádám, Gonda István, Orosz-Tóth Mihály, Kincses Sándorné, and Holb Imre
Plant nutrition significantly influences yield and fruit quality in fruit orchards. In this three-year study (2016–2018), different fertilizer treatments were compared in an intensive sweet cherry orchard. Trees of cultivar ‘Carmen’ were grafted on Prunus mahaleb ‘Cema’ rootstock, and were trained to free spindle. For NP, NPK and NPKMg treatments, yield ranged between 11.8 and 16.6 kg/tree in the three years, while the yield was 9.1 kg/tree on the control trees. Crop load (fruit amount calculated to the trunk thickness) was 151–166 g cm-2 for fertilized trees, while it was 120 g cm-2 on the untreated trees. Fruit sizes of fertilized trees reached 30 mm in 2018, while the fruit sizes of control trees were smaller with 2.5 mm. Water-soluble dry matter content (%) of the fertilized trees was lower in 2016 and 2017, but higher in 2018 compared to the control plots. In 2017 and 2018, fertilizer treatments resulted in an increase of the content of phosphorus (16–70%), potassium (4–22%) and magnesium (12–43%) in the fruits compared to control plots.