RESUMEN
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
A robust and dependable headspace HS-GC-MS method has been developed for the determination of carbon monoxide (CO) treated tuna fish. The performance of the method has been evaluated by analyzing spiked and blank samples. The proposed method uses a programmed temperature vaporizing (PTV) injector to implement the HS injection and overcome the negative effects on the column of water contained in the sample. The level of CO could be easily detected in the treated samples, its amount differing markedly from that detected in the untreated samples. Proper oven temperature programming prevented any deterioration of chromatographic performance caused by the accumulation of water, carbon dioxide and other low molecular weight hydrocarbons in the column during serial analyses. The introduction of PTV injection and the restoring of GC column, by oven temperature programming, were crucial for obtaining the required robustness. This procedure assures the run-to-run repeatability necessary for high throughput applications. The method affords linear calibration curves ranging from 50 to 2500 ng/g of CO content in tuna sample.
Asunto(s)
Monóxido de Carbono/análisis , Manipulación de Alimentos/métodos , Cromatografía de Gases y Espectrometría de Masas/métodos , Alimentos Marinos/análisis , Atún , Animales , Cromatografía de Gases y Espectrometría de Masas/instrumentación , Modelos Lineales , Reproducibilidad de los Resultados , TemperaturaRESUMEN
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
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 crystal structure of the title compound, C(18)H(13)NO(4), the oxidized form of the drug aminaftone used in venous disease therapy, is characterized by the presence of ribbons of hydrogen-bonded mol-ecules parallel to the [111] crystallographic direction and by stacking inter-actions between rings [centroid-centroid distance between quinone rings = 3.684â (3)â Å and between amino-benzoate rings = 4.157â (3)â Å] along the ribbons.
RESUMEN
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 general synthetic procedure leading to isotopomeric dihydro-2(3H)furanones (gamma-butyrolactones) containing two, four, or six deuterium atoms has been developed. The labeled dihydro-2(3H)furanones were synthesized in quantitative yield from the saturated diacid C4 (succinic) or unsaturated diacids C4 (fumaric, maleic, or acetylendicarboxylic) in the presence of Ru4H4(CO)8(PBu3)4 using a deuterium pressure of 180 bar at 180 degrees C. This methodology was applied to the total synthesis of a hexadeuterated matairesinol lignan: The 3,4-bis[[3-methoxy-4-(phenylmethoxy)phenyl]methyl]dihydro-2(3H)furanone-[7,7',8,8',9',9'-D6] (benzyl-protected matairesinol-D6) was fully characterized.
Asunto(s)
4-Butirolactona/química , Furanos/síntesis química , Marcaje Isotópico/métodos , Lignanos/síntesis química , Deuterio , Fumaratos/química , Maleatos/química , Rutenio , Ácido Succínico/químicaRESUMEN
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.