Quantitative Proton Magnetic Resonance Analysis of Primidone in Solid Dosage Forms

A rapid and specific proton magnetic resonance (PMR) spectroscopic method was developed for determining primidone in tablets. Maleic acid was used as the internal standart and DMSO-d₆ served as the PMR solvent.     

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.     

Quantitavive Proton Magnetic Resonance Analysis of Ranitidine in Solid Dosage Forms

A rapid and specific proton magnetic resonance (PMR) spectroscopic method was developed for determining ranitidine hydrochloride in tablets. 2-Choloroacetophenon was used as the internal standard and DMSO-d₆ served as the PMR solvent. The concentration of drug per unit dose was calculated from the integration values for the resonance signals of ranitidine hydrochloride at 4.32 δ ppm and int. st. at 5.19 δ ppm. The method using commercial products gave comparable results to those obtained by the methods of UV spectroscopy and USP XXIII.     

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.     

Near-Infrared Spectroscopy: Applications in the Analysis of Tablets and Solid Pharmaceutical Dosage Forms

Introduction

The popularity of near-infrared (near-IR) spectroscopy is rapidly increasing for many reasons. Availability of inexpensive yet powerful computers and chemometric software for spectral data analysis is fostering the growth of new applications of the technique. The development of rapid-scanning spectrometers offering very high signal-to-noise ratios, an increased understanding and acceptance of the method in a variety of industries, and the need to maintain real-time process control in an era of total quality management are other reasons this method has begun to receive such attention. Near-IR spectroscopy has been used for a wide range of analyses in industries as diverse as biomedicine and petrochemicals. Although the pharmaceutical industry has been relatively slow to embrace this technique, a variety of pharmaceutical applications of near-IR have been identified and investigated. This review will discuss the development of near-IR spectroscopy for the analysis of pharmaceutical dosage forms, specifically solid dosage from matrices, capsules, and tablets. The chemometric techniques used extensively in these analyses will also be discussed briefly.     

Quantitative Evaluation of the Lactate Signal Loss and Its Spatial Dependence in PRESS Localized H NMR Spectroscopy

Localized ¹H NMR spectroscopy using the 90°−t₁−180°−t₁+t₂−180°−t₂−Acq. PRESS sequence can lead to a signal loss for the lactate doublet compared with signals from uncoupled nuclei which is dependent on the choice of t₁ and t₂. The most striking signal loss of up to 78% of the total signal occurs with the symmetrical PRESS sequence (t₁=t₂) at an echo time of 2/J (290 ms). Calculations have shown that this signal loss is related to the pulse angle distributions produced by the two refocusing pulses which leads to the creation of single quantum polarization transfer (PT) as well as to not directly observable states (NDOS) of the lactate AX₃ spin system: zero- and multiple-quantum coherences, and longitudinal spin orders. In addition, the chemical shift dependent voxel displacement (VOD) leads to further signal loss. By calculating the density operator for various of the echo times TE=n/J, n=1, 2, 3, …, we calculated quantitatively the contributions of these effects to the signal loss as well as their spatial distribution. A maximum signal loss of 75% can be expected from theory for the symmetrical PRESS sequence and TE=2/J for Hamming filtered sinc pulses, whereby 47% are due to the creation of NDOS and up to 28% arise from PT. Taking also the VOD effect into account (2 mT/m slice selection gradients, 20-mm slices) leads to 54% signal loss from NDOS and up to 24% from PT, leading to a maximum signal loss of 78%. Using RE-BURP pulses with their more rectangular pulse angle distributions reduces the maximum signal loss to 44%. Experiments at 1.5 T using a lactate solution demonstrated a maximum lactate signal loss for sinc pulses of 82% (52% NDOS, 30% PT) at TE=290 ms using the symmetrical PRESS sequence. The great signal loss and its spatial distribution is of importance for investigations using a symmetrical PRESS sequence at TE=2/J.     

Two-Dimensional NMR Spectroscopy in Complete Analysis of the 1H and 13C NMR Spectra of the Ionophore A 23187 and its Calcium Salt

The complete assignment of the proton carbon spectra of the A 23187 Ionophore and its calcium salt is presented.     

Quantitative UV-Visible Diffuse Reflectance Spectroscopy of Solid Powders

In spite of difficulties in attaining high resolution, the determination of UV-VIS-NIR spectra via diffuse reflectance spectro-scopic measurements on solid powders; provides several advantages. Compounds which are difficult to obtain as suitable single crystals, or are found to be unstable or insoluble in liquid solution, can only be studied by diffuse reflectance spectroscopy. Also, since no solvents are required, any effects due to solvation are eliminated. However, it is not possible to resolve the observed spectrum into its anisotropic components, as in the case of single crystal spectra.     

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.     

Long Range Proton Couplings in Estrones

^4,6J_HH-long range couplings in an estrone-type molecule are observed and demonstrated to be helpful for the complete proton chemical shift assignment.     

核苷混合物的太赫兹谱定量分析

以物质的太赫兹吸收全谱为特征指纹可以进行混合物的成分分析。生化物质容易受外界影响而变性,使用光子能量只有毫电子伏特的太赫兹波来分析物质成分不会带来有害的电离辐射。文章使用太 赫兹谱成分分析法对腺苷、胸苷、鸟苷、胞苷、尿苷的混合物做了分析,实验结果表明该方法可以较为准确地分析出这几种核苷混合物的成分及其含量,相对误差在10%以内,并对误差产生的原因做了简 要分析。该项研究表明,此方法简单有效而且对样品无损。有可能成为生化物质成分分析的一种新手段,从而进一步拓展太赫兹谱的应用领域。     

Spectroscopy of light nuclei with skyrme-type interactions

Deformed Hartree-Fock calculations are performed for some light nuclei in a large configuration space consisting of first four major shells. The interaction employed is the modified Skyrme interaction in which the deformed density is replaced by the band averaged scalar density that makes the Hamiltonian rotationally invariant rendering the spectroscopic calculations feasible. It is shown that the introduction of density dependence spreads out the energy spectra and that the Skyrme variant SIV which has a weak density dependence gives best overall agreement for energy spectra and the available data for the electromagnetic properties of the nuclei studied. It is found that the maximum contribution to the energy of any state in the low lying spectrum comes from thes-state attractive ands-state repulsive parts of the Skyrme interaction. It is also shown that when two-body density dependent version of Skyrme interaction is used, the Koopmans theorem no longer holds.     

Identification and Quantitative Determination of Dipropylene Glycol in Terpene Mixtures Using 13C NMR Spectroscopy

A method that allows direct identification and quantitative determination of dipropylene glycol (DPG) using ¹³C NMR spectroscopy was developed. The quantitative procedure was checked and validated with commercially available DPG, controlled with two DPG-added essential oils, and then applied to commercial “Extraits de parfum” (perfume extracts).     

Derivative Spectroscopy in Conjunction with Thin Layer Chromatography Applied for Determination of Mixtures of Amino Acids in Baby Food.

The preparative thin layer chromatography using silica gel and solvent systems n. butanol : acetic acid: water (4:1:1 V/V) and 96% ethanol : water (70 : 30 v/v) were used to separate the amino acids mixture into groups that can be eluted and one or two of amino acids can be determined by derivative spectroscopy. This was done for determining histidine in presence of cystine, arginine in presence of lysine and ornithine, tryptophan in presence of tyrosine and phenylalanin, and methionine in presence of aspartic acid. The proposed method is applied for determination of these amino acids in baby food, Neslac, Dialac and Nestogen. The statistical analysis of the results were found to be good and in agreement with the ion exchange chromatographic method.     

显微激光诱导击穿光谱技术对低合金钢中Mn的定量检测

采用显微激光诱导击穿光谱技术对低合金钢标准样品进行定量分析,空间分辨率达到20 μm,单脉冲检测极限(LoD)为0.10%。根据谱线强度和元素浓度的关系获得Mn元素的基本定标曲线,定标曲线的拟合度系数R2为0.97,采用去一交互验证法预测了样品中Mn元素的浓度,七个样品的平均预测误差为12.91%,去一交互验证均方根误差为0.11%。采用内标法时定标曲线的拟合度系数R2为0.99,七个样品的平均预测误差为7.25%,去一交互验证均方根误差为0.07%。实验结果表明显微激光诱导击穿光谱技术能有效应用于物质微区元素的高精度定性、定量分析。     

Assignment of the 1H and 13C Spectra of 5-Methylthio-4H-1-(p-R1-phenyl)-3a-(p-R2-Phenyl)-3a, 4-dihydro (1,2,4) oxadiazolo(4,5-a), 1, 5-benzodiazepines Using 2D NMR Spectroscopy

The ¹H NMR spectra of the title benzodiazepines derivatives is highly congested because all the protons are in aromatic environment so many proton signals remain overlap even 300 MHz or higher fields. With this in mind, the assignment of the ¹H and ¹³C spectra of these compounds obtained using COSY, NOESY, HMQC and HMBC experiments is reported.     

Complete Analysis of the 1H and 13C NMR Spectra of 5-Isopropylsulfonyl-2-Norbornenes Through the Application of Two-Dimensional NMR Techniques

Total assignment of ¹³C and ¹H NMR spectra of the 5-isopropylsulfonyl-2-norbornenes 2 was achieved using the concerted application of two-dimensional homonuclear and heteronuclear chemical shift correlations. The stereochemistry of both the diastereoisomers endo 2a and exo 2b have been established using the magnitude of the proton coupling constants.     

Hyperfine Spectroscopy with Nuclear Resonant Scattering of Synchrotron Radiation

Since its observation in 1985 nuclear resonant scattering of synchrotron radiation has become an excellent tool to study hyperfine interactions in solids. It combines the advantages of both local probe experiments and scattering techniques and gives valuable information on magnetic and electronic structures in case of NFS experiments. Experiments benefit from the outstanding beam quality of 3rd generation synchrotron radiation sources, as the small beam size and divergence. This revised version was published online in August 2006 with corrections to the Cover Date.     

X射线荧光光谱法定性定量分析方法探讨

本文探讨了X射线荧光光谱法元素定性分析检出判定方法,并提出了一种与其他分析方法结合、利用荧光谱线强度比对对元素进行定量的单点外标法.方法简便、快速、实用,适用于大多数样品元素的分析.