Simultaneous Quantification of Aliskiren, Valsartan and Sitagliptin by LC with Fluorescence Detection: Evidence of Pharmacokinetic Interaction in Rats

A sensitive, precise and simple LC method for the simultaneous quantification of aliskiren, valsartan and sitagliptin in rat plasma has been developed and validated. The chromatographic separation was achieved on a C₁₈ column (250 mm × 4.6 mm, 5 μm) maintained at room temperature, using isocratic elution with acetonitrile/20 mM ammonium acetate buffer (35:65, v/v), pH adjusted to 4.85 with glacial acetic acid, and detected using a fluorescence detector. Liquid–liquid extraction of the aliskiren, valsartan and sitagliptin from the rat plasma with t-butyl methyl ether resulted in their high recoveries. LC calibration curves based on the extracts from the rat plasma were linear in the range of 25–2,000 ng mL^?1 for aliskiren and sitagliptin and 50–4,000 ng mL^?1 for valsartan. The limits of quantification were 25 ng mL^?1 for aliskiren and sitagliptin and 50 ng mL^?1 for valsartan. The precision and accuracy of the method were well within the generally accepted criteria for biomedical analysis. The described method was successfully applied to study the pharmacokinetics of aliskiren, valsartan and sitagliptin following oral administration, individually as well as in combination in Sprague–Dawley rats. The results of the study implied the occurrence of pharmacokinetic interaction upon the co-administration of these three drugs.     

Chemical composition and larvicidal activity of Zanthoxylum armatum against diamondback moth,Plutella xylostella

The diamondback moth, Plutella xylostella (L.) (Lepidoptera: Yponomeutidae) is the most serious pest of cruciferous crops grown in the world causing economic yield loss. Several synthetic insecticides have been used against P. xylostella but satisfactory control was not achieved due to development of resistance to insecticides. Therefore, the present study was carried out to screen different fractions of Zanthoxylum armatum for their insecticidal activities against second instar larvae of P. xylostella. Results indicate, all the fractions showed activity to P. xylostella. However, n-hexane fraction of Z. armatum showed maximum larvicidal activity with minimum LC₅₀ value of 2988.6 ppm followed by ethanol (LC₅₀ = 12779.7 ppm) and methanol fraction (LC₅₀ = 12908.8 ppm) whereas chloroform fraction was least toxic (LC₅₀ = 16750.6 ppm). The GC–MS analysis of n-hexane fraction of leaf extract showed maximum larvicidal activity, which may be due to two major compounds i.e. 2-undecanone (19.75%) and 2-tridecanone (11.76%).     

Zeta potential and electroosmotic mobility in microfluidic devices fabricated from hydrophobic polymers: 1. The origins of charge

This paper combines new experimental data for electrokinetic characterization of hydrophobic polymers with a detailed discussion of the putative origins of charge at water-hydrophobe interfaces. Complexities in determining the origin of charge are discussed in the context of design and modeling challenges for electrokinetic actuation in hydrophobic microfluidic devices with aqueous working fluids. Measurements of interfacial charge are complicated by slip and interfacial water structuring phenomena (see Part 2, this issue). Despite these complexities, it is shown that (i) several hydrophobic materials, such as Teflon and Zeonor, have predictable electrokinetic properties and (ii) electrokinetic data for hydrophobic microfluidic systems is most consistent with the postulate that hydroxyl ion adsorption is the origin of charge.     

Determination of aliphatic amines by high-performance liquid chromatography-amperometric detection after derivatization with naphthalene-2,3-dicarboxaldehyde

A simple and sensitive liquid chromatographic method has been developed for the determination of low molecular weight aliphatic amines after their pre-column derivatization with naphthalene-2,3-dicarboxaldehyde (NDA). Derivatization conditions, including the NDA concentration, reaction pH and reaction time have been investigated for method optimization. The chromatographic separation of five amines was performed on ABZ PLUS column using mobile phase of methanol-water (80:20, v/v) at a flow rate of 0.2 mL min⁻¹. The detection was carried out with a 6 mm glassy carbon electrode at the applied potential of 0.7 V versus Ag/AgCl reference electrode. The detection limits were between 23.3 and 34.4 nmol L⁻¹ of amines with a sample injection volume of 2 μL. The present method was applied for the determination of aliphatic amines in lake water. The recovery ranged 52.2-127.9%. The RSD in analytes retention time was less than 0.3% and 2.4% for intra- and inter-day analyses, respectively. The RSD in peak area was below 5.8% for both intra-day and inter-day analyses. The total analysis was completed within 20 min.     

Surface structural,morphological, and catalytic studies of homogeneously dispersed anisotropic Ag nanostructures within mesoporous silica

Highly dispersed anisotropic Ag nanostructures were synthesized within the channels of 3-aminopropyltrimethoxysilane (APTMS)-modified mesoporous SBA-15 for catalyzing the reduction of p-dinitrobenzene, p-nitrophenol, and p-nitroacetophenone, respectively. A green templating process without involving any reducing agent, by varying the amount (1–10 wt.%) of Ag loading followed by calcination at 350 °C under H₂ led to change in the morphology of Ag nanoparticles from nanospheres (~7–8 nm) to nanorods (aspect ratio ~12–30 nm) without any deformation in mesoporous sieves. In comparison to white bare SBA-15, gray-colored samples were formed with Ag impregnation exhibiting absorption bands at 484 and 840 nm indicating the formation of anisotropic Ag nanostructures within mesoporous matrix. TEM and FE-SEM micrographs confirmed the presence of evenly dispersed Ag nanostructures within as well as on the surface of mesoporous matrix. AFM studies indicated a small decrease in the average roughness of SBA-15 from 20.59 to 19.21 nm for 4 wt.% Ag/m-SBA-15, illustrating the encapsulation of majority of Ag nanoparticles in the siliceous matrix and presence of small amount of Ag nanoparticles on the mesoporous support. Moreover, due to plugging of mesopores with Ag, a significant decrease in surface area from 680 m²/g of SBA-15 to 385 m²/g was observed. The Ag-impregnated SBA-15 catalyst displayed superior catalytic activity than did bare SBA-15 with 4 wt.% Ag-loaded catalyst exhibiting optimum activity for selective reduction of p-nitrophenol to p-aminophenol (100 %), p-nitroacetophenone to p-aminoacetophenone (100 %), and p-dinitrobenzene to p-nitroaniline (87 %), with a small amount of p-phenylenediamine formation.

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Graphical abstract This paper demonstrates the spontaneous formation of uniformly dispersed Ag nanospecies of various morphologies (nanospheres, size ~7–8 nm and nanorods, aspect ratio ~12–30 nm), both within as well as on the surface of the mesoporous SBA-15, as a function of increased Ag loading. Surface structural and other physiochemical properties of Ag/m-SBA-15 nanocomposites were considerably influenced w.r.t change in Ag loading. Ag/m-SBA-15 nanocomposites with 4 wt.% Ag loading exhibited the highest selectivity (87 %) for the selective reduction of p-dinitrobenzene to p-nitroaniline and 100 % selectivity for p-nitrophenol to p-aminophenol and p-nitroacetophenone to p-aminoacetophenone, respectively.

     

Liquid–liquid extraction of thorium(IV) with N-n-heptylaniline from acid media

The extraction behavior of thorium(IV) from sulphuric acid medium with N-n-heptylaniline in xylene. Various parameters like reagent concentration, acid concentration, equilibration time, diverse ions and effect of diluents were studied. Thorium(IV) was selectively extracted and separated from many metal ions. The nature of the extracted species was determined. Thorium(IV) was analyzed from monazite ore and gas mantle.

     

Probing occurrence of phenylpropanoids in Morinda citrifolia in relation to foliar diseases

Accumulation of phenolic compounds in cell walls of different plant organs leading to increased lignification is an early defence response of plants against biotic stress. The aim of this work was to delineate occurrence of cell wall-bound (CWB) phenolic compounds in Morinda citrifolia leaves. Alkaline hydrolysis of the cell wall material of leaf tissues yielded 4-coumaric acid (4-CA) as the major bulk of the phenolic compounds in all Morinda germplasms. Next in line was 4-hydroxybenzoic acid. Other phenolics identified were vanillic acid, 4-hydroxybenzaldehyde, vanillin and ferulic acid. Concentrations of all the CWB phenolics were highest in the germplasm CHN-5, followed by the germplasm CHN-1. Incidentally, these two Morinda germplasms recorded lowest incidence of foliar diseases. Significantly higher amounts of 4-CA in combination with other phenolics may be the reasons for lowest incidence of foliar diseases in CHN-5 and CHN-1 germplasms of M. citrifolia.     

Particle interactions in kaolinite suspensions and corresponding aggregate structures

The surface charge densities of the silica face surface and the alumina face surface of kaolinite particles, recently determined from surface force measurements using atomic force microscopy, show a distinct dependence on the pH of the system. The silica face was found to be negatively charged at pH>4, whereas the alumina face surface was found to be positively charged at pH<6, and negatively charged at pH>8. The surface charge densities of the silica face and the alumina face were utilized in this study to determine the interaction energies between different surfaces of kaolinite particles. Results indicate that the silica face-alumina face interaction is dominant for kaolinite particle aggregation at low pH. This face-face association increases the stacking of kaolinite layers, and thereby promotes the edge-face (edge-silica face and edge-alumina face) and face-face (silica face-alumina face) associations with increasing pH, and hence the maximum shear-yield stress at pH 5-5.5. With further increase in pH, the face-face and edge-face association decreases due to increasing surface charge density on the silica face and the edge surfaces, and decreasing surface charge density on the alumina face. At high pH, all kaolinite surfaces become negatively charged, kaolinite particles are dispersed, and the suspension is stabilized. The face-face association at low pH has been confirmed from cryo-SEM images of kaolinite aggregates taken from suspension which show that the particles are mostly organized in a face-face and edge-face manner. At higher pH conditions, the cryo-SEM images of the kaolinite aggregates reveal a lower degree of consolidation and the edge-edge association is evident.     

Ambient pressure effects on the electrokinetic potential of Zeonor-water interfaces

Using phase-sensitive streaming potential experiments in a vacuum chamber, we demonstrate that lowering the ambient pressure of the air surrounding a hydrophobic, Zeonor microfluidic substrate results in a decrease in the time scale required for equilibration of the electrokinetic potential. At ambient air pressures below 0.74 atm, the electrokinetic potential changes from ～-84 mV to ～-11 mV in 5 h, while the same decrease occurs in a period of over 200 h when the system is at 1 atm. Returning a sub-atmospheric system (where the electrokinetic potential had equilibrated to -11 mV) to atmospheric pressure did not result in any additional change in the electrokinetic potential. This can be described as a type of hysteresis of the electrokinetic potential with dissolved gas concentration. No time or pressure dependence was observed for the electrokinetic potential of hydrophilic (silica) substrates.     

Ex-situ dispersion of core-shell nanoparticles of Cu-Pt on an in situ modified carbon surface and their enhanced electrocatalytic activities

Direct dispersion of core-shell nanoparticles on a carbon support (Cu@Pt/C) has been achieved while retaining the essential core-shell features of the nanoparticles by adopting an in situ surface modification-cum-anchoring strategy.