Validated Optimized Method for Simultaneous Analysis of Active Silymarin Components and Dimethyl-4,4′-dimethoxy-5,6,5′,6′-dimethylene Dioxybiphenyl-2,2′-dicarboxylate in a Pharmaceutical Preparation by Use of a Monolithic Silica C18 Column

A simple, rapid, and sensitive isocratic reversed-phase LC method using a monolithic column has been developed and validated for simultaneous analysis of the active components of silymarin [taxifolin, silydianin, silychristin, diastereomers of silybin (silybin A and B), and diastereomers of isosilybin (isosilybin A and B)] and dimethyl-4,4′-dimethoxy-5,6,5′,6′-dimethylene dioxybiphenyl-2,2′-dicarboxylate in a commercial formulation. The mobile phase was a 45:55 (v/v) mixture of methanol and 5 mM NaH₂PO₄ (adjusted to pH 2.75 with phosphoric acid) at a flow rate of 1.5 mL min^?1. UV detection was performed at 288 nm and quantification was based on peak area. The method was validated for linearity, accuracy, precision, selectivity, and robustness.     

Optimization and validation of an RP-HPLC method for direct determination of metformin hydrochloride in human urine and in a dosage form

A simple, selective, sensitive, accurate, and precise method was developed for determination of metformin hydrochloride (MF) in human urine using RP-HPLC. The method depends upon using an octylsilyl (C8) 5 microm particle size column at ambient temperature with mobile phase consisting of 33 mM sodium dihydrogen phosphate containing 6.38 mM hexanesulfonic acid sodium salt and adjusted to apparent pH 3.0 with phosphoric acid-acetonitrile (93 + 7, v/v) at a flow rate of 1.5 mL/min. Quantitation was achieved with UV detection at 231 nm based on peak area with a linear calibration curve over the concentration range of 0.01-50 microg/mL. The proposed method was applied to the determination of the urinary excretion pattern of MF (the cumulative amounts excreted were calculated without pretreatment of the urine sample) and for determination of the dissolution pattern of MF tablets. The proposed method was completely validated according to the U.S. Food and Drug Administration guidelines.     

Reflectance near-infrared spectroscopic method with Chemometric techniques for simultaneous determination of Chondroitin, glucosamine, and methyl sulfonyl methane

Reflectance near-IR (RNIR) spectroscopy was used for the simultaneous determination of chondroitin (CH), glucosamine (GO), and methyl sulfonyl methane (MSM) in tablets. Simple sample preparation was done by grinding, sieving, and compression of the tablets for improving RNIR spectra. Principal component regression and partial least squares (PLS-1 and PLS-2) were successfully applied to quantify the three components in the studied mixture using information included in RNIR spectra in the range of 4350-9100 cm(-1). The calibration model was developed with drug concentration ranges of 14.5-44.2% (w/w) for CH, 18.4-55.3% (w/w) for GO, and 6-18.6% (w/w) for MSM with addition of tablet excipients to the calibration set in the same ratio as in the tested tablets. The calibration models were evaluated by internal validation, cross-validation, and external validation using synthetic and pharmaceutical preparations. The proposed method was applied for analysis of six batches of the pharmaceutical product. The results of the proposed method were compared with the results of the pharmacopoeial method for the same batch of the pharmaceutical product. No significant differences between the results were found. The RNIR method is accurate and precise, and can be used for QC of pharmaceutical products.     

Utility of 2,3-dichloro-5,6-dicyano-p-benzoquinone in assay of codeine, emetine and pilocarpine

A simple and sensitive spectrophotometric method for the assay of codeine, emetine and pilocarpine is described, based on the interaction of these drugs (as n-electron donors) with 2,3-dichloro-5,6-dicyano-p-benzoquinone (as pi -acceptor) to give a highly coloured radical anion which exhibits maximum absorption at 460 nm. Formation of the radical anion has been established by electron spin resonance measurements. Beer's law is obeyed for the alkaloids investigated. The assay results are in accord with pharmacopoeial assay results. The procedure is sufficiently sensitive to permit unit dose assay of the individual alkaloids in pharmaceutical formulations.     

Reflectance near-infrared spectroscopic method with a chemometric technique using partial least squares multivariate calibration for simultaneous determination of chondroitin, glucosamine, and ascorbic acid

A reflectance near-infrared (RNIR) spectroscopy method was developed for simultaneous determination of chondroitin (CH), glucosamine (GO), and ascorbic acid (AS) in capsule powder. A simple preparation of the sample was done by grinding, sieving, and compression of the powder sample for improving RNIR spectra. Partial least squares (PLS-1 and PLS-2) was successfully applied to quantify the three components in the studied mixture using information included in RNIR spectra in the 4240-9780 cm(-1) range. The calibration model was developed with the three drug concentrations ranging from 50 to 150% of the labeled amount. The calibration models using pure standards were evaluated by internal validation, cross-validation, and external validation using synthetic and pharmaceutical preparations. The proposed method was applied for analysis of two pharmaceutical products. Both pharmaceutical products had the same active principle and similar excipients, but with different nominal concentration values. The results of the proposed method were compared with the results of a pharmacopoeial method for the same pharmaceutical products. No significant differences between the results were found. The standard error of prediction was 0.004 for CH, 0.003 for GO, and 0.005 for AS. The correlation coefficient was 0.9998 for CH, 0.9999 for GO, and 0.9997 for AS. The highly accurate and precise RNIR method can be used for QC of pharmaceutical products.     

New Luminescent Bioprobes Eu(lll)-phloroglucinol Derivatives and Their Spectrofluorimetric, Electrochemical Interactions with Nucleotides and DNA

Two new ligands derived from phloroglucinol 2-{[(4-methoxy benzoyl ) oxy ] } methyl benzoic acid[L1] and 2-{[(4-methyl benzoyl )oxy] methyl} benzoic acid[L2] were synthesized. The solid complex Eu(III)-L2 has been synthesised and characterized by elemental analysis ,UV and IR spectra. The reaction of Eu(III) with the two synthesized ligands has been investigated in I = 0.1 mol dm^-3 p-toluene sulfonate by cyclic voltammetry and square wave voltammetry. The reaction of Eu (III)–L1 and Eu (III)–L2 binary complexes with nucleotide 5′-AMP , 5′-ADP ,5′-ATP , 5′- GMP , 5′-IMP , and 5′-CMP has been investigated using UV, fluorescence and electrochemical methods. The experimental conditions were selected such that self-association of the nucleotides and their complexes was negligibly small, that is, the monomeric complexes were studied. The interaction of the Eu(III)–L1 or L 2 solid complexes with calf-thymus DNA has been investigated by fluorescence and electrochemical methods including cyclic voltammetery(CV) ,differential pulse polarography (DPP) and square wave voltammetry (SWV) on a glassy carbon electrode. The fluorescence intensity of Eu(III)-L2 complex was enhanced with the addition of DNA. Under optimal conditions in phosphate buffer pH 7.0 at 25 °C the linear range is 3–20 μM for calf thymus DNA (CT–DNA) and the corresponding determination limit is 1.8 μM.     

Strain-rate history and temperature effects on the torsional-shear behavior of a mild steel

Previous investigations on the effects of strain-rate and temperature histories on the mechanical behavior of steel are briefly reviewed. A study is presented on the influence of strain rate and strain-rate history on the shear behavior of a mild steel, over a wide range of temperature Experiments were performed on thin-walled tubular specimens of short gage length, using a torsional split-Hopkinson-bar apparatus adapted to permit quasi-static as well as dynamic straining at different temperatures. The constant-rate behavior was first measured at nominal strain rates of 10^?3 and 10³ s^?1 for ?150, ?100, ?50, 20, 200 and 400°C. Tests were then carried out, at the same temperatures, in which the strain rate was suddenly increased during deformation from the lower to the higher rate at various large values of plastic strain. The increase in rate occurred in a time of the order of 20 μs so that relatively little change of strain took place during the jump. The low strain-rate results show a well-defined elastic limit but no yield drop, a small yield plateau is found at room temperature. The subsequent strain hardening shows a maximum at 200°C, when serrated flow occurs and the ductility is reduced. The high strain-rate results show a considerable drop of stress at yield. The post-yield flow stress decreases steadily with increasing temperature, throughout the temperature range investigated. At room temperature and below, the strain-hardening rate becomes negative at large strains. The adiabatic temperature rise in the dynamic tests was computed on the assumption that the plastic work is entirely converted to heat. This enabled the isothermal dynamic stress-strain curves to be calculated, and showed that considerable thermal softening took place. The initial response to a strain-rate jump is approximately elastic, and has a magnitude which increases with decrease of testing temperature; it is little affected by the amount of prestrain. At 200 and 400° C, a yield drop occurs after the initial stress increment. The post-jump flow stress is always greater than that for the same strain in a constant-rate dynamic test, the strain-hardening rate becoming negative at large strains or low testing temperature. This observed effect of strain-rate history cannot be explained by the thermal softening accompanying dynamic deformation. These and other results concerning total ductility under various strain-rate and temperature conditions show that strain-rate history strongly affects the mechanical behavior of the mild steel tested and, hence, should be taken into account in the formulation of constitutive equations for that material.     

Semiclassical steady-state analysis of a degenerate two-photon laser

The steady-state analysis of a single-mode two-photon laser are treated semiclassically by using the Maxwell-Bloch equations. The theory is applied to a ring-laser model. We find similarities and significant differences between the one- and two-photon polarizations of the medium, population inversion and mode-pulling formula. The population inversion and the longitudinal variation of the steady-state modulus of the field are studied numerically. Received: 1 March 1999 / Received in final form: 8 April 1999     

Forecasting the impact of environmental stresses on the frequent waves of COVID19

Nonlinear Dynamics - A novel approach to link the environmental stresses with the COVID-19 cases is adopted during this research. The time-dependent data are extracted from the online repositories...     

Dy(III) complexes of metformin Schiff-bases as glucose probe: synthesis,spectral, and thermal properties

Complexes of Dy³⁺ with metformin-Schiff-bases of salicylaldehyde (HL¹); 2,3-dihydroxybenzaldehyde (H₂L²); 2,4-dihydroxybenzaldehyde (H₂L³); 2,5-dihydroxybenzaldehyde (H₂L⁴); 3,4-dihydroxybenzaldehyde (H₂L⁵); and 2-hydroxynaphthaldehyde (HL⁶) were synthesized by template reactions. The new compounds were characterized through elemental analysis, conductivity and magnetic moment measurements, IR, UV–vis, fluorescence, GC–MS, and XRD spectroscopies. The complexes are seven coordinate with formulas [DyL^1–4,6(NO₃)₂(H₂O)₂]·nH₂O where n?=?2, 2½, 4, 2, 2 and [DyL⁵(NO₃)(H₂O)₄]·2H₂O. TGA, DTG, and DTA analyses confirmed the suggested stereochemistry and subsequently the proposed mechanism of thermal decomposition. Kinetic and thermodynamic parameters were calculated for the second decomposition step. Thus, we report the ability of using the prepared complexes in the detection of glucose at physiological conditions using UV–vis and fluorescence spectroscopy as well as viscosity measurements, where the association constants were calculated.