RESUMEN
A novel method was set up with the aim to obtain a simultaneous cross comparative evaluation of different Gardenia Jasminoides Ellis fruits by the HPTLC fingerprint approach. The main components among the iridoid, hydroxycinnamic derivative and crocin classes were identified by TLC-MS ancillary techniques. The iridoids geniposide, gardenoside and genepin-1-ß-d-gentiobioside were also quantitated by densitometric scanning at 240nm. LiChrospher HPTLC Silica gel 60 RP-18 W F254, 20cm×10cm plates with acetonitrile: formic acid 0.1% (40:60 v/v) as the mobile phase was used. The method was validated giving rise to a dependable and high throughput procedure well suited to routine applications. Iridoids were quantified in the range of 240-1140ng with RSD of repeatability and intermediate precision between 0.9-2.5% and accuracy with bias 1.6-2.6%. The method was tested on six commercial Gardenia Jasminoides fruit samples.
Asunto(s)
Cromatografía en Capa Delgada/métodos , Frutas/química , Gardenia/química , Iridoides/análisis , Espectrometría de Masas/métodos , Iridoides/químicaRESUMEN
A novel HPTLC-densitometric method was developed for separation and quantitation of primulasaponin I and II in different matrices. HPTLC silica gel 60 F254(S), 20 cm × 10 cm, plates with ethyl acetate:water:formic acid (5:1:1 v/v) as the mobile phase were used. Densitometric determinations were performed in reflectance mode at 540 nm after derivatization with vanillin reagent. The method was validated giving rise to a dependable and high throughput procedure well suited to routine applications. Primulasaponins were quantified in the range of 150-450 ng with RSD of repeatability and intermediate precision between 0.8 and 1.4% and accuracy within the acceptance limits. The method was tested on commercial herbal medicinal preparations claiming to contain primula root extract.
Asunto(s)
Cromatografía en Capa Delgada , Preparaciones de Plantas/análisis , Raíces de Plantas/química , Primula/química , Saponinas/análisis , Acetatos/química , Benzaldehídos/química , Calibración , Cromatografía en Capa Delgada/normas , Densitometría , Formiatos/química , Plantas Medicinales , Estándares de Referencia , Reproducibilidad de los Resultados , Gel de Sílice/química , Agua/químicaRESUMEN
A new HPTLC method was envisaged to determine rosmarinic acid (RA) in different matrices with the aim of testing the influence of optimizing the main HPTLC operative parameters in view of a more stringent validation process. HPTLC LiChrospher silica gel 60 F254s, 20 cm × 10 cm, plates with toluene:ethyl formate:formic acid (6:4:1, v/v) as the mobile phase were used. Densitometric determinations were performed in reflectance mode at 330 nm. The method was validated giving rise to a dependable and high throughput procedure well suited to routine applications. RA was quantified in the range of 132-660 ng with RSD of repeatability and intermediate precision not exceeding 2.0% and accuracy within the acceptance limits. The method was tested on several commercial preparations containing RA in different amounts.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Cromatografía Líquida de Alta Presión/normas , Cromatografía en Capa Delgada/métodos , Cromatografía en Capa Delgada/normas , Cinamatos/análisis , Depsidos/análisis , Reproducibilidad de los Resultados , Ácido RosmarínicoRESUMEN
A novel method based on the fluorescence excited solely on aloin by a H3BO3 derivatizing procedure, allowed its rapid and selective determination among the co-occurring components in a variety of complex matrices as several Aloes dried extracts and related commercial products. HPTLC LiChrospher silica gel 60 F254S, 20 cm x 10 cm, plates with ethyl formate: CH3OH:H2O (100:14.5:10, v/v) as the mobile phase were used. Densitometric determinations were performed in fluorescence mode, exciting wavelength 365 nm, optical filter K540 after derivatization with H3BO3. The method was validated giving rise to a dependable and high throughput procedure well suited to routine application. Aloin was quantified in the range of 110-330 ng with RSD of repeatability and intermediate precision not exceeding 2.3% and accuracy inside the acceptance limits.
Asunto(s)
Cromatografía en Capa Delgada/métodos , Emodina/análogos & derivados , Espectrometría de Fluorescencia/métodos , Ácidos Bóricos/química , Calibración , Densitometría/métodos , Emodina/análisis , Emodina/química , Ensayos Analíticos de Alto Rendimiento , Estructura Molecular , Estándares de Referencia , Reproducibilidad de los Resultados , Soluciones , Factores de TiempoRESUMEN
The overall mol-ecular geometry of the title compound, C(11)H(12)N(4)O(3)S, is bent, with a dihedral angle of 89.24â (5)° between the best planes through the two aromatic rings. Each mol-ecule behaves as a hydrogen-bond donor toward three different mol-ecules, through its amidic and the two aminic H atoms, and it behaves as a hydrogen-bond acceptor from two other mol-ecules via one of its sulfonamidic O atoms. In the crystal, mol-ecules linked by N-Hâ¯N and N-Hâ¯O hydrogen bonds form kinked layers parallel to (001), adjacent layers being connected by van der Waals inter-actions.
RESUMEN
The physico-chemical and structural characterization of diacerhein, an anthraquinone with antiinflammatory activity, employed in the symptomatic treatment of inflammatory osteoarthritis, is reported. The combined use of FT-IR, DSC, X-ray powder and single-crystal diffraction has provided a valuable tool to fully characterize the title compound. The X-ray diffraction study has revealed the existence of hydrogen-bond assisted tight packing of the quasi-planar molecules in the solid. The collected results are intended to implement the information required for the compilation of drug master files.
Asunto(s)
Antraquinonas/química , Antiinflamatorios no Esteroideos/química , Cristalización , Cristalografía por Rayos X , Análisis Diferencial Térmico , Enlace de Hidrógeno , Conformación Molecular , Estándares de Referencia , Espectroscopía Infrarroja por Transformada de Fourier , ComprimidosRESUMEN
Metoprolol, a widely used adrenoreceptor blocking drug, is commonly administered as the succinate or tartrate salt. The structure of metoprolol succinate, C(15)H(26)NO(3) (+)·0.5C(4)H(4)O(4) (2-), is characterized by the presence of ribbons in which cations, generated by N-protonation of the metoprolol mol-ecules, are hydrogen bonded to succinate anions. The dicarboxylic acid transfers its H atoms to two metoprolol mol-ecules; the asymmetric unit contains one cation and half an anion, the latter possessing twofold rotational symmetry. There are localized nets of O-Hâ¯O and N-Hâ¯O hydrogen bonds along a ribbon, within centrosymmetric arrangements formed by pairs of metoprolol cations and pairs of anions, each of the latter contributing with one of its carboxyl groups to the localized net. This arrangement is repeated along the ribbon by the operation of the twofold axis bis-ecting the anion, as well as by the lattice translation.
RESUMEN
The structure [Danilovski et al. (2001 â¶). Croat. Chim. Acta74, 103-120] of the T-N (non-solvated) polymorph of torasemide, C(16)H(20)N(4)O(3)S, a diuretic drug used in the treatment of hypertension, has been redetermined at low temperature. The zwitterionic form of the mol-ecule is confirmed, although GAUSSIAN03 calculations suggest that this form is less stable in the gas phase. The unit-cell contraction between 298 and 100â K is approximately isotropic and the largest structual change is in a C-N-C-C torsion angle, which differs by 11.4â (3)° between the room-temperature and low-temperature structures. There are two mol-ecules in the asymmetric unit, both of which contain an intra-molecular N-Hâ¯N hydrogen bond. In the crystal structure, both mol-ecules form inversion dimers linked by pairs of N-Hâ¯N hydrogen bonds. Further N-Hâ¯N and N-Hâ¯O hydrogen bonds lead to a three-dimensional network. The different hydrogen-bond arrangements and packing motifs in the polymorphs of torasemide are discussed in detail.
RESUMEN
The title compound, C(16)H(20)N(4)O(3)S·0.25CH(4)O·0.25H(2)O, is a hydrate/methanol solvate of torasemide, a diuretic drug used in the treatment of hypertension. The asymmetric unit contains two torasemide mol-ecules and half-occupied methanol and water mol-ecules. It is isomorphous with the previously reported nonsolvated T-II form of torasemide. The water mol-ecules contribute to the stability of the structure by participating in an extensive system of O-Hâ¯O hydrogen bonds; N-Hâ¯N and N-Hâ¯O hydrogen bonds are also present. Both asymmetric mol-ecules of torasemide form inversion dimers in the crystal.
RESUMEN
The validation of a HPTLC-densitometric method for the determination of secoisolariciresinol diglucoside (SDG) in flaxseed was performed improving the reproducibility of a previously reported HPTLC densitometric procedure by the use of fully wettable reversed phase plates (silica gel 60 RP18W F(254S), 10cmx10cm) with MeOH:HCOOH 0.1% (40:60, v/v) mobile phase. The analysis required only the alkaline hydrolysis in aqueous medium of undefatted samples and densitometry at 282nm of HPTLC runs. The method was validated following the protocol proposed by the Société Francaise des Sciences et Techniques Pharmaceutiques (SFSTP) giving rise to a dependable and high throughput procedure well suited to routine application. SDG was quantified in the range of 321-1071ng with RSD of repeatability and intermediate precision not exceeding 3.61% and accuracy inside the acceptance limits. Flaxseed of five cultivars of different origin was elected as test-bed.
Asunto(s)
Butileno Glicoles/análisis , Cromatografía en Capa Delgada/métodos , Lino/química , Glucósidos/análisis , Butileno Glicoles/química , Densitometría/métodos , Glucósidos/químicaRESUMEN
The structure of the title compound, C(14)H(28)N(3)O(2) (+)·HSO(4) (-), a nootropic drug (pramiracetam) investigated for cognition-enhancing properties, is closely similar to that of the previously determined acetonitrile solvate, both structures being characterized by the presence of ribbons of hydrogen-bonded ions. The pyrrolidine ring adopts an envelope conformation.
RESUMEN
A novel stability-indicating high-performance liquid chromatographic (HPLC) method was developed and validated for the assay of diacerhein in bulk forms. Diacerhein was found to degrade in alkaline and acidic conditions and also under oxidative stress. The drug was stable to dry heat and in presence of light. Resolution of drug, its potential impurities and degradation products were achieved on a RP18 (endcapped) column utilizing 0.1 M phosphoric acid and methanol (40:60, v/v) as eluent at the detection wavelength of 254 nm. The validation studies were carried out fulfilling International Conference on Harmonisation (ICH) requirements. The procedure was found to be specific, linear, precise (including intermediate precision), accurate and robust.
Asunto(s)
Antraquinonas/análisis , Antiinflamatorios no Esteroideos/análisis , Cromatografía Líquida de Alta Presión/métodos , Estabilidad de Medicamentos , Antraquinonas/química , Antiinflamatorios no Esteroideos/química , Calibración , Química Farmacéutica/métodos , Cromatografía , Contaminación de Medicamentos , Concentración de Iones de Hidrógeno , Espectrometría de Masas , Metanol/farmacología , Modelos Químicos , Estrés Oxidativo , Preparaciones Farmacéuticas/análisis , Ácidos Fosfóricos/farmacología , Control de Calidad , Sensibilidad y Especificidad , Espectrofotometría Ultravioleta , Tecnología Farmacéutica/métodos , Factores de TiempoRESUMEN
A HPTLC-densitometric method, based on an external standard approach, was developed in order to obtain a novel procedure for routine analysis of secoisolariciresinol diglucoside (SDG) in flaxseed with a minimum of sample pre-treatment. Optimization of TLC conditions for the densitometric scanning was reached by eluting HPTLC silica gel plates in a horizontal developing chamber. Quantitation of SDG was performed in single beam reflectance mode by using a computer-controlled densitometric scanner and applying a five-point calibration in the 1.00-10.00 microg/spot range. As no sample preparation was required, the proposed HPTLC-densitometric procedure demonstrated to be reliable, yet using an external standard approach. The proposed method is precise, reproducible and accurate and can be employed profitably in place of HPLC for the determination of SDG in complex matrices.