Identification of Phenothiazine Derivatives and Analogs by X-Ray Diffraction. II. Active Substances in Pharmaceutical Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 633-639
Author(s):  
A De Leenheer ◽  
A Heyndrickx
Keyword(s):  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Pharmaceutical Formulations ◽  
X Ray Diffraction ◽  
Phenothiazine Derivatives ◽  
X Ray ◽  
Diffraction Patterns ◽  
Related Compounds ◽  
Active Substances

Abstract Procedures have been developed for the isolation of phenothiazines and chemically related compounds from pharmaceutical formulations, namely, injections, solutions, tablets, coated tablets, creams, sirups, lotions, and suppositories. In general, active substances are crystallized as picrates. A few compounds, however, gave better crystalline derivatives as free bases (levomepromazine and propericiazine), quaternary ammonium salt (thiazinamium), or chlorhydrate salts (amitriptyline and nortriptyline). The crystalline derivatives prepared were specifically identified by comparison of their Debye-Scherrer X-ray diffraction patterns with those for reference compounds obtained under the same conditions.

The two solid-state conformations of nefopam methiodide, a quaternary ammonium salt of the analgesic drug

1990 ◽  
Vol 68 (7) ◽  
pp. 1128-1134 ◽  
Author(s):  
Robert Glaser ◽  
André Michel ◽  
Marc Drouin
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Analgesic Drug ◽  
X Ray ◽  
Positional Disorder ◽  
X Ray Crystallography

The solid-state structure of nefopam methiodide, a quaternary ammonium salt of nefopam hydrochloride (a non-narcotic analgesic drug), has been determined by single crystal X-ray diffraction analysis. Nefopam methiodide gives crystals belonging to the monoclinic P21/c space group and, at 298 K, a = 10.001(1), b = 9.928(1), c = 17.598(1) Å, β = 94.41(1)°, V = 1742.2(2) Å3, Z = 4, R(F) = 0.086, and Rw(F) = 0.108. Due to disorder, the boat (flattened chair) and twist-chair (flattened chair) conformations of the 2,5-benzoxazocine eight-membered ring were both observed in the crystal with 55:45 occupancy, respectively. Positional disorder was also observed for the iodide counterion, which showed occupancies of 81:9.5:9.5. Keywords: nefopam, analgesic, X-ray crystallography, conformation.

Identification of Crystalline Derivatives of Butyrophenones by X-Ray Diffraction: Examination of Pure Compounds and Active Substances in Pharmaceutical Formulations

1971 ◽  
Vol 54 (6) ◽  
pp. 1406-1419
Author(s):  
E Okkerse ◽  
A De Leenheer ◽  
A Heyndrickx
Keyword(s):  
Diffraction Data ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
X Ray Diffraction ◽  
Photographic Recording ◽  
X Ray ◽  
Pure Compounds ◽  
Diffraction Patterns ◽  
Derivatives Of ◽  
Active Substances

Abstract Isolation and crystallization procedures have been developed for butyrophenones as free substances and from pharmaceutical formulations, namely ampoules, coated tablets, drops, and tablets. Crystallization as free bases, picrates, picrolonates, chlorhydrates, bromates, sulfates, and phosphates was attempted for all compounds. For the crystalline derivatives, the X-ray diffraction data were obtained by the Debye-Scherrer powder technique with photographic recording. The products have been classified according to their X-ray data, using “Hanawalt’s three strongest lines index” and the “innermost line index” systems. The butyrophenones could be identified with certainty by direct comparison of the X-ray diffraction patterns of compounds isolated from dosage forms with reference patterns.

Organophilization of Four Differents Bentonitic Clays with a Quaternary Ammonium Salt

2005 ◽  
Vol 498-499 ◽  
pp. 67-72 ◽  
Author(s):  
Daniela de Lourdes A.C.S. Andrade ◽  
Wildemberg A. Freire ◽  
Sueila S. Araújo ◽  
Lucianna G.F. Vieira ◽  
Ana Cristina Figueiredo de Melo Costa ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Drilling Fluids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimethyl Benzyl ◽  
Dimethyl Benzyl Ammonium ◽  
Petroleum Drilling

Organophilic Bentonities clays are widely used for industrial purposes, as components of petroleum drilling fluids as well as in cosmetics, lubricants adhesives and paints. Most recent they have been used as fillers in polymer nanocomposites. In this work, three organophilic bentonitic clays from the distric of Boa Vista and one from Campina Grande, PB, Brazil, were synthesized and characterized. The four clays were treated with a quaternary chloride ammonium salt- dimethyl benzyl ammonium alkyl chloride (Dodigen 1611) provided by Chemco. The cation exchange and swelling capacities of the modified clays were determined and the clays were characterized by FTIR, Thermal Analysis (DTA, TGA) and X-ray diffraction. The results showed the modification of all four clays by the quaternary ammonium salt to be successful.

Reversible phase transformation-type layer shape electrolyte based on POM and quaternary ammonium salt

2014 ◽  
Vol 07 (02) ◽  
pp. 1450019 ◽  
Author(s):  
Xuefei Wu ◽  
Yunyan Li ◽  
Qingyin Wu ◽  
Hong Ding ◽  
Wenfu Yan
Keyword(s):  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Water Solution ◽  
X Ray Diffraction ◽  
Inorganic Layer ◽  
X Ray ◽  
Type Layer ◽  
Transformation Type ◽  
Reversible Phase

A novel kind of organic–inorganic layer shape material, polyoxymetalates (POM)-type ionic liquid (IL) with Keggin structure and simple quaternary ammonium salt, (TOAMe)4PW11VO40 (trioctylmethylammonium = TOAMe,…) is synthesized and characterized by IR, UV, X-ray diffraction (XRD), TG–DTA. Its electrochemical property was investigated by cyclic voltammgram. Research results released the vanadium and the POM structure in the compound can process reduction in DMSO, which is unlikely in water solution as a simple hydrated ion because water will protonize substrate.

Influence of Clay Incorporation on the Physical Properties of Polyethylene/Brazilian Clay Nanocomposites

2008 ◽  
Vol 8 (4) ◽  
pp. 1937-1941
Author(s):  
R. Barbosa ◽  
E. M. Araújo ◽  
T. J. A. Melo ◽  
E. N. Ito ◽  
E. Hage
Keyword(s):  
Mechanical Properties ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Dispersion Analysis ◽  
Clay Nanocomposites ◽  
X Ray Diffraction ◽  
Clay Particles ◽  
Transmission Electron ◽  
The Matrix

High density polyethylene/Brazilian clay nanocomposites were prepared by the melt intercalation technique. A montmorillonite sample from Boa Vista/PB, Northeast of Brazil, was organically modified with esthearildimethylammonium chloride (Praepagen WB) quaternary ammonium salt. The unmodified and modified clays with the quaternary ammonium salt were introduced in 1, 2, 3 and 5 wt% in a PE polymer matrix. The dispersion analysis and the interlayer distance of the clay particles were obtained by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The mechanical properties of tensile and the flammability of the nanocomposites were studied. In general, the mechanical properties of the systems presented superior values compared to the matrix. The systems showed a reduction on the burning rate, indicating that the flammability resistance of nanocomposites was improved.

scholarly journals THERMAL BEHAVIOR OF PARACETAMOL AND TABLETS OF REFERENCE, GENÉRIC AND SIMILAR

2012 ◽  
Vol 09 (17) ◽  
pp. 28-37
Author(s):  
Francisca Edivânia MORAIS ◽  
Sheila Pricila Marques CABRAL ◽  
Eliane Gonçalves ARAUJO ◽  
Carlos Alberto MARTINEZ-HUITLE ◽  
Nedja Suely FERNANDES
Keyword(s):  
Particle Size ◽  
Thermal Behavior ◽  
Pharmaceutical Formulations ◽  
Endothermic Peak ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermoanalytical Techniques ◽  
Diffraction Patterns ◽  
Dsc Curves

The present study utilized the thermoanalytical techniques (TG, DTG, DTA and DSC) to evaluate the thermal behavior of tablets containing paracetamol and marketed as reference, generic and similar. The samples were also characterized by IR, X-ray diffraction and SEM. The TG/DTG curves presented similar behaviour indicanting a low influence of the excipients present in pharmaceutical formulations. The DTA and DSC curves showed an endothermic peak between about 165.0 and 195.0 oC characteristic of melting of paracetamol in all samples. The X-ray diffraction patterns showed similarities and characterized the compounds as crystallines. The micrographs indicated heterogeneity in particle size.

Identification of Phenothiazine Derivatives and Analogs by X-Ray Diffraction. I. Examination of Pure Compounds

1971 ◽  
Vol 54 (3) ◽  
pp. 625-632 ◽  
Author(s):  
A De Leenheer ◽  
A Heyndrickx
Keyword(s):  
Diffraction Data ◽  
Reference Data ◽  
X Ray Diffraction ◽  
Phenothiazine Derivatives ◽  
Photographic Recording ◽  
Index Method ◽  
X Ray ◽  
Pure Compounds ◽  
Related Compounds

Abstract X-ray diffraction data for phenothiazines and chemically related compounds have been obtained by the Debye-Scherrer powder technique with photographic recording. Classification of compounds according to their X-ray data has been made, using the “innermost line index” method. The results obtained serve as reference data with absolute specificity for identification purposes.

scholarly journals LiCrO2 Under Pressure: In-Situ Structural and Vibrational Studies

Crystals ◽  
2018 ◽  
Vol 9 (1) ◽  
pp. 2 ◽  
Author(s):  
Alka Garg ◽  
Daniel Errandonea ◽  
Julio Pellicer-Porres ◽  
Domingo Martinez-Garcia ◽  
Swayam Kesari ◽  
...  
Keyword(s):  
Research Work ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pressure Coefficients ◽  
Vibrational Studies ◽  
Diffraction Patterns ◽  
The Stability ◽  
Murnaghan Equation ◽  
Related Compounds

The high-pressure behaviour of LiCrO2, a compound isostructural to the battery compound LiCoO2, has been investigated by synchrotron-based angle-dispersive X-ray powder diffraction, Raman spectroscopy, and resistance measurements up to 41, 30, and 10 Gpa, respectively. The stability of the layered structured compound on a triangular lattice with R-3m space group is confirmed in all three measurements up to the highest pressure reached. The dependence of lattice parameters and unit-cell volume with pressure has been determined from the structural refinements of X-ray diffraction patterns that are used to extract the axial compressibilities and bulk modulus by means of Birch–Murnaghan equation-of-state fits. The pressure coefficients for the two Raman-active modes, A1g and Eg, and their mode-Grüneisen parameters are reported. The electrical resistance measurements indicate that pressure has little influence in the resistivity up to 10 GPa. The obtained results for the vibrational and structural properties of LiCrO2 under pressure are in line with the published results of the similar studies on the related compounds. Research work reported in this article contributes significantly to enhance the understanding on the structural and mechanical properties of LiCrO2 and related lithium compounds.

scholarly journals Surface Adsorption Properties and Layer Structures of Homogeneous Polyoxyethylene-Type Nonionic Surfactants in Quaternary-Ammonium-Salt-Type Amphiphilic Gemini Ionic Liquids with Oxygen- or Nitrogen-Containing Spacers

Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 4881
Author(s):  
Risa Kawai ◽  
Maiko Niki ◽  
Shiho Yada ◽  
Tomokazu Yoshimura
Keyword(s):  
Surface Tension ◽  
Ionic Liquids ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
Nonionic Surfactants ◽  
Alkyl Chain ◽  
Surface Adsorption ◽  
X Ray ◽  
Layer Structures

The amphiphilic ionic liquids containing an alkyl chain in molecules form nano-structure in the bulk, although they also show surface activity and form aggregates in aqueous solutions. Although insights into the layer structures of ionic liquids were obtained using X-ray and neutron scattering techniques, the nanostructures of ionic liquids remain unclear. Herein, the surface adsorption and bulk properties of homogeneous polyoxyethylene (EO)-type nonionic surfactants (CxEO6; x = 8, 12, or 16) were elucidated in quaternary-ammonium-salt-type amphiphilic gemini ionic liquids with oxygen or nitrogen-containing spacers [2Cn(Spacer) NTf2; (Spacer) = (2-O-2), (2-O-2-O-2), (2-N-2), (2/2-N-2), (3), (5), or (6); n = 10, 12, or 14 for (2-O-2) and n = 12 for all other spacers] by surface tension, small- and wide-angle X-ray scattering, cryogenic transmission electron microscopy, and viscosity measurements. The surface tension of C12EO6 in 2Cn(Spacer) NTf2 with oxygen-containing spacers increased with increasing concentration of C12EO6, becoming close to that of C12EO6 alone, indicating that the amphiphilic ionic liquid adsorbed at the interface was replaced with CxEO6. In contrast, both 2Cn(Spacer) NTf2 with nitrogen-containing spacers and nonionic surfactants remained adsorbed at the interface at high concentrations. In the bulk, it was found that 2Cn(Spacer) NTf2 formed layer structures, in which the spacing depended on the alkyl chain length of CxEO6. These insights are expected to advance the practical applications of amphiphilic ionic liquids such as ion permeation, drug solubilization, and energy delivery systems.

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