A fast capillary electrophoretic method is described for the separation and determination of the enantiomers of the novel wake-promoting agent, modafinil. Several parameters affecting the separation were studied, including the type and concentration of chiral selector, buffer pH, buffer concentration, voltage and temperature. Good chiral separation of the racemic mixture was achieved in less than 5 min with resolution factor Rs?=?2.51, using a bare fused-silica capillary and a background electrolyte (BGE) of 25 mM H3PO4?1 M tris solution; pH 8.0; containing 30 mg mL?1 of sulfated-β-cyclodextrin (S-β-CD). The separation was carried out in normal polarity mode at 25 ?C, 18 kV and using hydrostatic injection. Acceptable validation criteria for selectivity, linearity, precision, and accuracy were included. The developed method was successfully applied to the assay of enantiomers of modafinil in pharmaceutical formulations. The computational calculations for the enantiomeric inclusion complexes rationalized the reasons for the different migration times between the modafinil enantiomers. 相似文献
The objectives of this investigation were to establish a validated stability-indicating LC method for assay of carvedilol and to study the degradation behaviour of the drug under different ICH-recommended stress conditions. Chromatographic separation was achieved on a C18 column with 55:45 (%, v/v) acetonitrile–0.02 m phosphate buffer, pH 3.5, as mobile phase at a flow rate of 1.0 mL min?1; detection was by UV absorbance at 242 nm. The method was validated for linearity, precision, accuracy, robustness, specificity, and sensitivity, with the bulk drug. The drug was subjected to forced degradation and peaks of all the degradation products were well resolved from that of the pure drug, with significantly different retention times, which indicates the specificity and stability-indicating properties of the method. First-order degradation kinetics of carvedilol were observed under acidic and alkaline conditions. When the utility of the method was verified by analysis of the drug in marketed tablets and a nano-emulsion formulation, the assay was found to be 98.60–99.61 and 99.52–99.87, respectively. These results indicate the method can be successfully used for routine analysis of carvedilol in the bulk drug and in pharmaceutical dosage forms. 相似文献
Selective polymeric extractants were prepared for preconcentration of Cibacron reactive red dye, a dye that is often applied
with Cibacron reactive blue and Cibacron reactive yellow for dyeing of fabrics. The best extractant was fabricated (in chloroform)
using methacrylic acid (as monomer), ethylene glycol dimethacrylate (as crosslinker), AIBN (as initiator for polymerization),
and red dye as template molecule, with a molar stoichiometric ratio of 8.0:40.0:2.5:0.63, respectively. The structure of the
molecularly imprinted polymer (MIP) was robust, and resisted dissolution up to 260 °C. Compared with the un-imprinted polymer,
the imprinted product has a large specific surface area which improved its adsorption capacity. The effect of imprinting was
obvious from the adsorption capacity measured at pH 4 for red dye (the imprinted molecule), which was increased from 24.0
to 79.3 mg g−1 after imprinting. Equilibrium adsorption studies revealed that the dye-imprinted-polymer enables efficient extraction of
red dye even in the presence of blue and yellow dyes which have similar chemical natures to the red dye. The selectivity coefficients
Sred dye/dye, were 13.9 and 17.1 relative to the yellow and blue dyes, respectively. The MIP was found to be effective for red dye preconcentration,
with a preconcentration factor of 100, from tap water and treated textile wastewater. The factors affecting extraction of
red dye by the MIP were studied and optimized. Under the optimized extraction conditions, red dye was selectively quantified
in the presence of other competing dyes at a concentration of 20 μg L−1 from different water systems with satisfactory recoveries (91–95%) and RSD values (∼5.0%). 相似文献
Lycopene is a potent antioxidant that has been shown to play critical roles in disease prevention. Efficient assays for detection and quantification of lycopene are desirable as alternatives to time- and labor-intensive methods. Attenuated total reflectance infrared (ATR-IR) spectroscopy was used for quantification of lycopene in tomato varieties. Calibration models were developed by partial least-squares regression (PLSR) using quantitative measures of lycopene concentration from liquid chromatography as reference method. IR spectra showed a distinct marker band at 957 cm(-1) for trans Carbon-Hydrogen (CH) deformation vibration of lycopene. PLSR models predicted the lycopene content accurately and reproducibly with a correlation coefficient (sigma) of 0.96 and standard error of cross-validation <0.80 mg/100 g. ATR-IR spectroscopy allowed for rapid, simple, and accurate determination of lycopene in tomatoes with minimal sample preparation. Results suggest that the ATR-IR method is applicable for high-throughput quantitative analysis and screening for lycopene in tomatoes. 相似文献
This numerical study describes the eddy emergence and transformations in a slow steady axisymmetric air–water flow, driven by a rotating top disk in a vertical conical container. As water height \(H_{\mathrm{w}}\) and cone half-angle \(\beta \) vary, numerous flow metamorphoses occur. They are investigated for \(\beta =30^{\circ }, 45^{\circ }\), and \(60^{\circ }\). For small \(H_{\mathrm{w}}\), the air flow is multi-cellular with clockwise meridional circulation near the disk. The air flow becomes one cellular as \(H_{\mathrm{w}}\) exceeds a threshold depending on \(\beta \). For all \(\beta \), the water flow has an unbounded number of eddies whose size and strength diminish as the cone apex is approached. As the water level becomes close to the disk, the outmost water eddy with clockwise meridional circulation expands, reaches the interface, and induces a thin layer with anticlockwise circulation in the air. Then this layer expands and occupies the entire air domain. The physical reasons for the flow transformations are provided. The results are of fundamental interest and can be relevant for aerial bioreactors. 相似文献
Herein we report the successful implementation of the consecutive and simultaneous photodissociation with high (213 nm) and low (10.6 μm) energy photons (HiLoPD, high-low photodissociation) on ubiquitin in a quadrupole-Orbitrap mass spectrometer. Absorption of high-energy UV photon is dispersed over the whole protein and stimulates extensive C–Cα backbone fragmentation, whereas low-energy IR photon gradually increases the internal energy and thus preferentially dissociates the most labile amide (C–N) bonds. We noticed that simultaneous irradiation of UV and IR lasers on intact ubiquitin in a single MS/MS experiment provides a rich and well-balanced fragmentation array of a/x, b/y, and z ions. Moreover, secondary fragmentation from a/x and z ions leads to the formation of satellite side-chain ions (d, v, and w) and can help to distinguish isomeric residues in a protein. Implementation of high-low photodissociation in a high-resolution mass spectrometer may offer considerable benefits to promote a comprehensive portrait of protein characterization.
Lead sulfate is produced when a lead acid battery discharges, and it is also known that big PbSO4 crystals are less active than the smaller ones because they dissolve slower, thus result in failure of the battery. However, little is known if chemically prepared PbSO4 can be used as active material of lead acid batteries. Here, we report the preparation of PbSO4 by facile chemical precipitation of aqueous lead acetate with sodium sulfate and its utilization as the positive active material. The results show that the PbSO4 alone is not good enough for the purpose, but its mixtures with Pb3O4 are as excellent as the industrial leady oxide. For example, the mixtures containing 5, 10, 20, and 30 wt.% of Pb3O4 discharge 78.2, 92.9, 88.0, and 91.5 mAh g?1 at a current density of 100 mA g?1, respectively. Also, the one with 10 % Pb3O4 remains 93 % capacity in 150, 100 % DOD cycles. 相似文献
The propagation of linear and nonlinear electrostatic waves is investigated in a magnetized anisotropic electron-positron-ion (e-p-i) plasma with superthermal electrons and positrons. A two-dimensional plasma geometry is assumed. The ions are assumed to be warm and anisotropic due to an external magnetic field. The anisotropic ion pressure is defined using the double adiabatic Chew-Golberger-Low (CGL) theory. In the linear regime, two normal modes are predicted, whose characteristics are investigated parametrically, focusing on the effect of superthermality of electrons and positrons, ion pressure anisotropy, positron concentration and magnetic field strength. A Zakharov-Kuznetsov (ZK) type equation is derived for the electrostatic potential (disturbance) via a reductive perturbation method. The parametric role of superthermality, positron content, ion pressure anisotropy and magnetic field strength on the characteristics of solitary wave structures is investigated. Following Allen and Rowlands [J. Plasma Phys. 53, 63 (1995)], we have shown that the pulse soliton solution of the ZK equation is unstable to oblique perturbations, and have analytically traced the dependence of the instability growth rate on superthermality and ion pressure anisotropy. 相似文献