Quantitative Analysis of Acetazolamide in Solid Dosage Forms with 1H-Nmr Spectroscopy

A rapid and specific proton magnetic resonance spectroscopic method was developed for determining acetazolamide in tablets. Maleic acid was used as the internal standard and DMSO-d₆ served as the NMR solvent. the concentration of drug per unit dose was calculated from the integration values for the resonance signals of acetazolamide at 2.14 ppm and maleic acid at 6.20 ppm. the method using commercial products gave comparable results of those obtained by the method of USP XXIII.     

Proton scattering from unstable nuclei

Recent improvements in the intensities and optical qualities of radioactive beams have made possible the study of elastic and inelastic proton scattering on unstable nuclei. The design and performances of an innovative silicon strip detector array devoted to such experiments are described. The quality of the data obtained are illustrated with recent results obtained at the GANIL facility for unstable oxygen, sulfur and argon isotopes. Methods to analyse the data using phenomenological and microscopic optical model potentials are discussed.     

Long Range 13C Couplings in Hexamethylphosphoramide and Dimethylsulphoxide

One bond ¹³C–¹H couplings have been extensively studied and their magnitudes explained on the basis of two contributing factors, namely the percentage “s” character of the bond¹ and the carbon Z value, or effective nuclear charge². To date however, little has been reported on ¹³C couplings over more than one bond, the main reason being the previous experimental difficulties in measuring these small couplings.     

NMR Study of Pentafluoroaniline - Hydrogen Bonding and Proton Exchange

The temperature and concentration dependence of ¹H NMR chemical shifts of pentafluoroaniline and aniline in acetone (Ac), dimethylsulphoxide (DMSO) and hexamethylphosphortriamide (HMPA) indicate that the effect of hydrogen bond formation, δ = δ_obs - δ_A' is similar for both anilines. The analysis of ¹H NMR spectra showed, that proton exchange of t-butyl alcohol (tBA) and 2,6-di-t-butylphenol (DTBPh) with pentafluoroaniline is slower than that with aniline.     

Intramolecular Hydrogen Bonding in Bilirubin Monomethyl Esters Determined by 1H-NMR Spectroscopy

Analysis of the N-H ¹H-NMR chemical shifts of the monomethyl esters of bilirubin-IIIα, IXα and XIIIα reveals a preference in CDCl₃ for folded conformations in which the unesterified propionic acid carboxyl group is intramolecularly H-bonded to the opposing pyrromethenone unit. The remaining pyrromethenone unit may be weakly intramolecularly H-bonded to the propionic ester carbomethoxy group.     

Intermolecular Hydrogen Bonding and Dimeric Structures in Bilirubin Esters from 1H-NMR Spectroscopy

Analysis of the N-H ¹H-NMR chemical shifts of various bilirubin dimethyl esters indicates intermolecularly H-bonded dimers in CDCl₃ solution with pairwise pyrromethenone associations. The presence of an exo (C-2 or C-18) vinyl or ethyl group on the lactam ring leads to relatively weaker H-bonding as compared with an endo (C-3 or C-17) vinyl or ethyl group. Consequently, in a non-symmetric bilirubin, e.g. IXα, the endo-vinylpyrromethenone to endo-vinylpyrromethenone intermolecular H-bonding becomes much stronger (with more deshielded N-H proton chemical shifts) than in corresponding symmetric isomers, e.g. XIIIα or IIIα.     

The Proton NMR Assignment of 1-Aminocyclo-propane-1-carboxylic Acid

The two sets of diastereomeric hydrogen atoms cis and trans to the carboxylate of 1-aminocyclopropane-1-carboxylic acid (ACC) were differentiated by a ¹H-nmr study. The measurement of the ¹H-nmr spectrum of ACC at pH 3.8 during the successive addition of non-chiral lanthanide reagents such as Eu(NO₃)₃, Pr(NO₃)₃ or Gd(NO₃)₃ demonstrated that the hydrogen atoms cis to the carboxylate function of ACC resonate at δ=1.42 and that the hydrogen atoms trans to the carboxylate function of ACC resonate at δ=1.20. The mono-substituted cyclopropanes, cyclo-propanecarboxylic acid (CPC) and cyclopropyl-amine (CPA) were used in complementary lanthanide-reagent shift titrations along with the back titration of an ACC-Eu⁺⁺⁺ complex with DCl to further substantiate the assignment. This assignment allows for the non-destructive, nonisotopic diluting analysis of various biosynthetically derived deuterated ACC's formed from the corresponding deuterated S-adenosyl-L-methionine.     

UV, 1H NMR Studies and a Semiempirical Mo Calculations of Some Substituted Phenylthiomethyl Benzoic Acid Derivatives

The effect of substituents on the spectral behavior of some arylthiomethyl benzoic acid derivatives, the corresponding sulfoxides and sulfones were studied. The chemical shifts of ortho hydrogen of benzyl moieties gave linear correlations with Hammett constants for acid sulfides and concave curves for sulfide esters. The effect of substituents on the conformation of sulfides were discussed.     

In Vitro Study of Ketoprofen and Indapamide Used in Multidrug Therapy: 1H-NMR Analysis

ABSTRACT

Interaction of ketoprofen (KP, a nonsteroidal anti-inflammatory drug) and indapamide (IDP, a thiazide-related diuretic) with human serum albumin (HSA) in low-affinity binding sites (LAS) and competition between these medicines used in multidrug therapy have been studied by proton nuclear magnetic resonance (¹H-NMR) spectroscopy.

The analysis of chemical shifts, Δσ (ppm), of drug proton resonances and the values of the association constant, K_a [M^?1], were used to estimate the effect of IDP and KP on the KP–HSA and IDP–HSA complexes, respectively. The results showed the changes in the affinity of human serum albumin toward the drug with different mechanisms of action (KP and IDP) and the competition in the binding to HSA.     

Proton and Carbon - 13 NMR Assignments for Fluorinated and Nonfluorinated Aromatic Ketimines

The ¹H and ¹³C NMR spectra of three aromatic ketimines with varying degrees of fluoro substitution have been extensively studied using one and two dimensional techniques. COSY experiments were conducted to identify the protons on each of the aromatic groups, HETCORR experiments were then utilized to identify the corresponding carbon atoms, and then the order of the carbon atoms was established by long-range HETCORR (HRTCORRLR) results. These studies have allowed rigorous assignments to be made for most of the carbon and hydrogen atoms present in these compounds. Fluorine splittings were very helpful in the analyses. In the course of this study, the NMR absorbances (¹H and ¹³C) of related aldimines have also been assigned. This constitutes the first report on the assignments of ¹H and ¹³C absorbances for ketimines. The observed spectral properties suggest that the structure of aromatic ketimines is one in which the aromatic rings are in three different planes. Two of the aromatic rings, the N-substituted ring and the C-substituted ring in the cis configuration, are twisted substantially out of the plane with respect to the -C=N- bond. The remaining C-substituted aromatic ring, trans to the N-substituted ring, lies in the deshielding zone of the imine bond.     

Spectroscopic Investigation of the Antazoune-p-chloranilic Acid Reaction Product

Spectroscopic studies on the reaction of p-chloranilic acid with antazoline base are reported. These include UV/VIS and IR spectrophotoraetry, electron spin resonance (ESR) and nuclear magnetic resonances (¹H-NMR & ¹³C-NMR). The results reveal that the antazoline-p-chloranilic acid product is an ion pair salt rather than a charge-transfer complex.     

Determination of Internucleotide JHN Couplings by the Modified 2D JNN-Correlated [N, H] TROSY

Recent developments in the direct observation of J couplings across hydrogen bonds in proteins and nucleic acids provide additional information for structure and function studies of these molecules by NMR spectroscopy. A J_NN-correlated [¹⁵N, ¹H] TROSY experiment proposed by Pervushin et al. (Proc. Natl. Acad. Sci. USA 95, 14147–14151, 1998) can be applied to measure ^hJ_HN in smaller nucleic acids in an E.COSY manner. However, it cannot be effectively applied to large nucleic acids, such as tRNA^Trp, since one of the peaks corresponding to a fast relaxing component will be too weak to be observed in the spectra of large molecules. In this Communication, we proposed a modified J_NN-correlated [¹⁵N, ¹H] TROSY experiment which enables direct measurement of ^hJ_HN in large nucleic acids.     

Matrix Lie Algebras and Integrable Couplings

Three kinds of higher-dimensional Lie algebras are given which can be used to directly construct integrable couplings of the soliton integrable systems. The relations between the Lie algebras are discussed. Finally, the integrable couplings and the Hamiltonian structure of Giachetti-Johnson hierarchy and a new integrable system are obtained, respectively.     

Integrable Couplings of the Coupled Burgers Hierarchy

In this letter, a new loop algebra G is constructed, from which a new isospectral problem is established. It follows that integrable couplings of the well-known coupled Burgers hierarchy are obtained.     

Lie Algebras for Constructing Nonlinear Integrable Couplings

Two new explicit Lie algebras are introduced for which the nonlinear integrable couplings of the Giachetti-Johnson (GJ) hierarchy and the Yang hierarchy are obtained, respectively. By employing the variational identity their Hamiltonian structures are also generated. The approach presented in the paper can also
provide nonlinear integrable couplings of other soliton hierarchies of evolution equations.     

Integrable Couplings of Classical-Boussinesq Hierarchy and Its Hamiltonian Structure＊

By using a Lie algebra, an integrable couplings of the classicai-Boussinesq hierarchy is obtained. Then, the Hamiltonian structure of the integrable couplings of the classical-Boussinesq is obtained by the quadratic-form identity.     

Structural Elucidation of the Hitherto 2,3-Dihydro-1,2,3,5-Benzothiatriazepine-1,1-Dioxide Ring System1,2

The structure of the product from the successive reaction of pyridinium 2-benzamido-5-chloro-4-methylbenzenesulfonate with PCl₅ and excess anhydrous hydrazine has been established as 8-chloro-4-phenyl-7-methyl-2,3-dihydro-1,2,3,5-benzothiatriazine-1,1-dioxide, 1. MS, IR, ¹H and ¹³C NMR have provided definite proof of 1.     

The Double Integrable Couplings of Tu Hierarchy

Two types of Lie algebras are presented, from which two integrable couplings associated with the Tu isospectral problem are obtained, respectively. One of them possesses the Hamiltonian structure generated by a linear isomorphism and the quadratic-form identity. An approach for working out the double integrable couplings of the same integrable system is presented in the paper.     

A Low Frequency H-NMR External Unit for the Analysis of Large Foodstuff Samples

An inexpensive external unit that allows the use of a commercial high-resolution NMR spectrometer as a very low frequency instrument is described. The external unit is phase coherent, the pulse timing being given by the parent spectrometer. With the exception of the probe, the external unit does not contain any tuned elements. This permits easy change of frequency in the range 100 kHz–1 MHz. The external unit may be appropriately employed in food science where, in several cases, low frequency is desirable. An application to hen shell eggs at the frequency of 700 kHz is described.     

Generalized Two-State Theory for an Atom Laser with Nonlinear Couplings

We present a generalized two-state theory to investigate the quantum dynamics and statistics of an atom laser with nonlinear couplings. The rotating wave approximate Hamiltonian of the system is proved to be analytically solvable. The fraction of output atoms is then showed to exhibit an interesting collapse and revival phenomenon with respect to the evolution time, a sign of nonlinear couplings. Several nonclassical effects, such as sub-Poissonian distribution, quadrature squeezing effects, second-order cross-correlation and accompanied violation of Cauchy-Schwartz inequality are also revealed for the output matter wave. The initial global phase of the trapped condensate, in weak nonlinear coupling limits, is found to exert an interesting impact on the quantum statistical properties of the propagating atom laser beam.