Authors:Ishita A. Basera, Aboli Girme, Vijay P. Bhatt, Ganesh Saste, Sandeep Pawar, Lal Hingorani, and Mamta B. Shah
A validated UHPLC-PDA with an ESI-MS/MS method has been developed for simultaneous estimation of six bioactive alkaloids (magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine) in the different extracts of the roots of Berberis aristata DC (Family:Berberdiaceae). It is an important medicinal herb native to Northern Himalaya and commonly known as ‘daruharidra’, ‘daruhaldi’, ‘Indian barberry’ or ‘tree turmeric’. An insight into the research literature uncovered reports on isoquinoline alkaloids like magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine, and berberine as major bioactives in B. aristata roots, possessing different pharmacological and therapeutic effects. In the present study, these aforementioned alkaloids were separated on Phenomenex Luna®, 5 µm-C8 analytical column. The HPLC-MS analysis was performed at a flow rate of 0.90 mL min−1. Each alkaloid that is resolved was characterized by precursor ions and fragment ions with electrospray ionization (ESI) source in both positive and negative ionization using scan mode. The limit of detections (LODs) were 0.087, 0.727, 0.035, 0.124, 0.782 and 0.794 μg mL−1 for magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine, respectively. The proposed UHPLC-PDA method was fully validated according to international (ICH) guidelines and was found to be selective, sensitive and highly accurate for the concomitant estimation of the aforementioned symbolic bio-markers of B. aristata roots.
Authors:Hemanth Kumar Chanduluru and Abimanyu Sugumaran
The current study explores a design and development of the simple, fast, green and selective novel method of UPLC to quantify pitavastatin and ezetimibe simultaneously. The combined approach of Green Analytical Method with Quality by Design-based risk assessment was done using the Ishikawa fishbone diagram followed by a rotatable central composite design used for the optimization. The optimal chromatographic separation was attained through a mobile phase of 72: 28% v/v ethanol and 0.1% orthophosphoric acid (pH 3.5), with a 0.31 mL min−1 flow rate. The developed UPLC-PDA method was sensitive and specific for pitavastatin and ezetimibe, with linearity ranging from 2 to 30, 10–150 μg mL−1 with an R2 of 0.9999 and 0.9997, respectively. The forced degradation study of stability-indicating assay results shows the degradation in respective stress conditions. The developed UPLC method was validated and found to have sensible results with good linearity, accuracy and precision. Further, the greenness was evaluated using five states of art metrics like NEMI, GAPI, AES, AMGS, and AGREE metrics and found the greenest results. Based on the results we concluded that the developed UPLC method could be efficient for the simultaneous determination of pitavastatin and ezetimibe in bulk and tablet dosage.
Authors:Farsang Andrea, Barta Károly, Szatmári József, and Bartus Máté
Kutatásunk során Magyarország két dél-alföldi réti csernozjom talajú területét vizsgáltuk azon céllal, hogy in situ körülmények között számszerűsítsük a különböző szélesemények által okozott talajveszteség mértékét, az ezzel együtt járó humusz- és tápanyagáthalmozás nagyságrendjét, valamint a két terület defláció érzékenységében tapasztalt különbségek okait.
Vizsgálati területeink Békés megyében, Makótól K-re mintegy 10 km-re, Apátfalva külterületén, valamint Csongrád megyében Szegedtől ÉNy-ra 2 km-re helyezkedtek el. Kutatásunk célkitűzései az alábbiak voltak: terepi szélcsatornás mérésekre alapozott laboratóriumi mérések alapján különböző szerkezeti állapotú csernozjom talajokra meghatározni
◾a szélerózióval áthalmozott szedimentben mért makroelem, és humuszanyag feldúsulását,
◾valamint az ezekre ható talajtani tényezőket.
A hasonló mechanikai összetételű, Szeged és Apátfalva melletti réti csernozjom talajok aggregátum összetételében, valamint a CaCO3 és humusztartalomban megfigyelhető különbségek hatására a Szeged melletti csernozjom mintaterület talaja defláció érzékenyebb. A Szegedtől É-ra eső csernozjomokon 6,5–9,0 m s–1 közötti indítósebesség értékeket mértünk, míg Apátfalván 13,0 m s–1 volt az indítósebesség értéke. Az apátfalvi terület talajának magasabb karbonát- és humusztartalma, valamint aggregátum összetételében mért magasabb morzsa arány az indítósebességérték növelésének irányába hat. A feltalajban a 0,5 mm-nél kisebb aggregátumok magasabb aránya következtében nemcsak kisebb indítósebesség értékeket, hanem nagyobb áthalmozódó talajmennyiséget, valamint ezzel együtt nagyobb mennyiségű humusz- és foszfor elmozdulást mértünk az egységesen 10-10 perces fújatási kísérleteink alkalmával a szegedi mintaterületen. Megállapítható tehát, hogy egyazon talajtípusba eső, s azonos textúrájú (homokos vályog) talajok esetében az aggregátum összetételben, valamint a CaCO3 és humusztartalomban megfigyelhető eltérések hatására jelentős különbségek tapasztalhatók a defláció érzékenység, az indítósebesség, a szediment szállítás módja és a humusz- és elemáthalmozás mértéke között.
In our research, two Chernozem soil areas were examined in the southern part of the Great Hungarian Plain in order to quantify the amount of the soil loss, humus and nutrient transport caused by different wind events and in order to show the causes of the differences in the sensitivity of deflation between the two areas.
Our study areas were located in Békés County, one of them was near Apátfalva, about 10 km east of Makó, and the other one was 2 km northeast of Szeged in Csongrád County. Our in situ wind tunnel experiments were accomplished on 2–4 June 2011 at Apátfalva and in July 2013 in Szeged. The objectives of our research were the followings:
◾determination of the enrichment ratios for humus, macro- and microelements in the wind eroded sediments in the case of Chernozem soils with different structures based on field experiments and laboratory measurements;
◾determination the affecting actual soil factors;
◾estimation of soil loss and element rearrangement trends on Chernozem arable lands under different wind velocity on plot scale.
Because of the differences in the aggregate size distribution, CaCO3 and humus content, Chernozem soil near Szeged is more sensitive to deflation than near Apátfalva. Threshold friction velocity was measured between 6.5 and 9.0 m s–1 near Szeged, while the same parameter was 13.0 m s–1 at Apátfalva. The higher carbonate and humus content and the higher crumb ratio of the soil on the Apátfalva area result increasing threshold friction velocity. Due to the higher proportion of aggregates smaller than 0.5 mm in the topsoil, we have measured not only lower threshold friction velocities, but also a larger quantity of transported soil and a larger humus and phosphorus loss during the uniform 10-10 minute long wind tunnel experiments in the Szeged sample area. It can be concluded that even in spite of the same soil type and same texture there are significant differences between deflation sensitivity, threshold friction velocity, sediment transport mode, humus and nutrient transportation because of the significant differences in aggregate size distribution, CaCO3 and humus content.
It means that the agronomic structure of the soils greatly influences the mitigation and aggravation of the soil the stress effects caused by climate change. Extreme weather situations have drawn attention to the fact that improperly applied cultivation methods, tools, and overuse of Chernozem soils can modify the soil structure. One of the most serious affect is the dusting of the surface layer of the soil. During this process the larger macroaggregates disintegrate into microaggregates and the resulting smaller fractions are more exposed to wind erosion.
The dust load affecting our settlements is mainly originated from arable lands. The mitigation of this emission is fundamentally based on the regulation of land use, farming practices and deflation. “Best Management Practices” (BMPs) mean a group of selected tools that can reduce or eliminate the transport of pollutants from diffuse sources before, during and/or after agricultural activities. However, these diffuse agricultural loads caused by wind erosion can only be quantified if the magnitude and spatial movement of the dust and pollutants is monitored.
Authors:Chen Chen, Jingjing Li, Feng Xiong, Bo Wang, Yuanming Xiao, and Guoying Zhou
Anisodus tanguticus (Maxim.) Pascher is an important Tibetan folk medicine and the source of tropane alkaloids (TAs) grown in Qinghai-Tibet Plateau. There are marked differences in quality of A. tanguticus from geographic areas. The aim of present research was to establish a method for the quantitative analysis of TAs coupled with chemometrics analysis to trace geographical origins. Qualitative analysis of TAs in A. tanguticus was carried out using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and quantitative analysis of TAs in different plant organs from different geographical origin was achieved. Contents of TAs were subjected to the principal component analysis, and orthogonal partial least-squares discriminant analysis. The contents of the three marker compounds (anisodamine, anisodine and atropine) in the roots and acrial parts of A. tanguticus were positive correlated and varied significantly from different geographical origins. Principal component analysis, and orthogonal partial least-squares discriminant analysis results showed excellent discrimination between different geographical origin of A. tanguticus. This study could provide comprehensive evaluation and further utilization of A. tanguticus resources.
Authors:Joliana F. Farid, Nadia M. Mostafa, Hebatallah M. Essam, and Yasmin M. Fayez
Due to the wide applicability of separation techniques that rely on the property of differential migration in pharmaceutical formulations analysis, different analytical strategies have been proposed to resolve mixtures of multi-components pharmaceuticals. Three separation methods were developed and validated for the simultaneous determination of Paracetamol (PAR), Pseudoephedrine HCl (PSE) and Chlorpheniramine maleate (CHP). The first method is a thin-layer chromatographic (TLC) separation, followed by densitometric measurement. The separation was carried out on aluminium sheet of silica gel 60 F254 using ethanol:chloroform:ammonia (1:7:0.4, by volume) as the mobile phase. Determination of PAR, PSE and CHP was successfully applied over the concentration ranges of 3–25 µg/band, 0.5–10 µg/band and 0.1–6 µg/band, respectively. The second method is HPLC separation that was achieved on C18 column using the mobile phase acetonitrile:phosphate buffer pH 5 (10:90, v/v) at a flow rate 1 mL min−1. PAR, PSE and CHP were determined by HPLC in concentration ranges of 5–400 μg mL−1, 2–40 μg mL−1 and 0.5–16 μg mL−1, respectively. The third method is a capillary electrophoresis (CE) separation. The electrophoretic separation was achieved using 20 mM phosphate buffer (pH 6.5) at 20 kV. The linearity was reached over concentration ranges of 30–250 μg mL−1, 5–50 μg mL−1 and 0.8–20 μg mL−1 for PAR, PSE and CHP, respectively. The developed methods were validated with respect to linearity, precision, accuracy and system suitability. The proposed methods were successfully applied for bulk powder and dosage form analysis with RSD of precision <2%. Moreover, statistical comparison with the official methods confirms the methods' validity.
Authors:Maha A.M. El-Shazly, Ahmed A. Hamed, Hoda A. Kabary, and Mosad A. Ghareeb
The therapeutical applications of ornamental plants have been categorized to be of a great effectiveness in multiple industries from ancient times until present days. Pluchea dioscoridis is widely known Egyptian wooden plant that has been extensively applied for different medicinal purposes. In this study, LC-ESI-MS/MS analysis of the potent antimicrobial ethyl acetate and n-butanol extracts of P. dioscoridis leaves led to identification of 28 and 21 compounds, respectively. The identified compounds were categorized as phenolic acids, phenolic acids derivatives, organic acids, flavonoids (aglycones and glycosides), secoiridoids, coumarin derivatives, and gallotannins derivatives. Among them, caffeic acid 3-sulfate was the most predominate in the investigated extracts followed by ferulic acid and dicaffeoyl-quinic acid. Also, the antimicrobial potentiality of different extracts was evaluated against different pathogenic microbes including Enterobacter cloacae, Micrococcus leutus, Aeromonas hydrophila, Bacillus subtilis, Bacillus cereus, Bacillus lichneformis and Clostridium species. Furthermore, different concentrations of the most potent extract were assayed for antibacterial efficacy on growth curve kinetics against the susceptible bacteria along 4days incubation period. Our gathered data confirmed that, the antimicrobial activity against tested bacteria was different according to the solvent used in the extraction process. Mostly, all the extracts showed a wide spectrum antibacterial activity except the plant water extract which shows a mild activity against Clostridium sp. only. Based on the highest inhibition zone diameter, the ethyl acetate extract followed by butanol extract exhibited the highest inhibition zone with Micrococcus luteus and B. subtilis (20.0 and 18.5 mm) respectively. Determining the effect of ethyl acetate extract at different concentration (0, 0.66, 1.66, 3.33, 6.67, 13.34 and 20.01 mg mL−1) on M. luteus growth kinetics, the data assured that the antibacterial activity shows concentration dependent manner with the highest antibacterial activity at 20.01 mg mL−1 culture. The data also confirmed that, none of the selected concentration showed bactericidal activity in the prepared cultures, and with the prolonged incubation period the bacteria acquire resistance against the extract beginning from second or third day of incubation.
Authors:Anikó Lambert-Meretei, Eszter Vozary, and Timea Kaszab
In the case of fruit syrups, consumers prefer thicker, deep-coloured ones because they remind them of good old homemade ones. Physical properties – as viscosity, colour, refractive index, soluble solid content (SSC), and electrical impedance - of fruit syrups flavoured with raspberry or orange juice were determined. The change of the measured physical properties was determined in three different experiments: 1. evaluating the effect of sugar and sweetener content 2. evaluating the effect of fruit juice composition and 3. evaluating the effect of sugar content on syrups containing raspberry or orange juice only. Variations in fruit and sugar content had a definite effect on the physical properties of squashes. Viscosity, SSC value, refractive index, and impedance magnitude increased with increasing sugar content and decreased with replacement of sugar with sweeteners although colour characteristics were defined mostly by the colorant added to the squash. Changes in the fruit composition of syrups could influence viscosity, refractive index, and SSC values but the magnitude of impedance showed little changes for all samples. The characteristics of squashes containing only raspberry or orange juice and different sugar content did not follow any trends, which emphasized that additives had a significant effect on the physical properties.
Authors:Jelena Dzudovic, Milkica Crevar Sakac, Marko Antunovic, Aleksandra Repic, Slobodan Obradovic, Snezana Djordjevic, Jelena Savic, and Boris Dzudovic
Oral anticoagulants are a group of drugs used for the prevention and treatment of venous thrombosis and venous thromboembolism. For the last ten years, direct oral anticoagulants (DOAC) have been available and are equally effective, but significantly safer than vitamin K antagonists. In the case of an overdose, their most important side effect is still bleeding. Due to their widespread use, as well as increased toxicological importance there is a need to develop an analytical method for the determination of DOAC in biological material.
The aim of this paper was to establish a method for the quantification of apixaban as one of the representatives of DOAC. The methodology of the study included the measurement of apixaban in the plasma of patients treated in the intensive care unit. Plasma apixaban concentrations were determined by LC-MS/MS technique using carbamazepine as an internal standard. Obtained validation parameters indicate that the introduced method is sensitive, reliable, precise and accurate. Using this method, apixaban can be quickly and easily detected and quantified in plasma in patients who are suspected of overdosing with this drug.
A sweeping micellar electrokinetic chromatography (sweeping-MEKC) method was developed for the determination of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. Several parameters affecting sweeping-MEKC method were studied systematically and the separation conditions were optimized as 20 mM NaH2PO4–110 mM SDS and 40% (v/v) MeOH (pH 2.4), with −22 kV applied voltage and UV detection at 230 nm. The sample matrix is 60 mmol L−1 NaH2PO4 and sample introduction was performed at 3 psi for 6 s. Separation of the four naphthalenediols was completed in less than 17 min. Limit of detection (LOD) and limit of quantitation (LOQ) are 0.0045∼0.0094 μg mL−1 and 0.015∼0.031 μg mL−1. Linear relationship (r2 > 0.999) is satisfactory at the range of 0.1–10 μg mL−1. The developed method has been successfully applied to the determination of the four naphthalenediols in real cosmetic samples, with recoveries in foundation, sun cream and lotion in the range of 92.3%∼106.8% and relative standard deviation (RSD) less than 4.15%. A HPLC method described in the National Standards of the People’s Republic of China was carried out for the comparison with the proposed method. The results showed that the proposed sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.
Napping is one of the rapid sensory profiling methods, which was established recently to meet the needs of sensory and consumer researchers. This approach provides a holistic evaluation of the tested sample through their positioning in a 2-dimensional space. The protocol of the analysis is somewhat different from the traditionally applied descriptive methods, like Quantitative Descriptive Analysis. In our review, we focus on the applicability of Napping in the field of fermented goods. The accompanying procedures are also investigated (typically Flash Profiling, CATA, and further methods), in order to understand how the combined datasets facilitate the understanding of the sensory characteristics of the products.