[Research on TLC identification and anti-coagulant activity quantitatively methods of Scolopendra subspinipes mutilans].

OBJECTIVE: To improve the quality standard of Scolopendra subspinipes mutilans by researching the methods of the TLC identification and anti-coagulant activity quantitatively. METHODS: Identified the free arginine (Arg) and serine (Ser) in scolopendra by TLC, screened the samples preparation process and developed solvent systems; Determined the anti-coagulant activity by method of titration with thrombin and screened the pretreatment methods. RESULTS: When medicinal materials was extracted by formic acid and 95% ethanol (1:1) with ultrasonic method and developed by n-butanol-acetic acid-water (12:5:4), the spots of Arg and Ser were well separated. Ultrasonic method was suitable for preparation of the anti-coagulant components in Scolopendra subspinipes mutilans and their anti-coagulant activity was determined by method of titration with thrombin could get a well reproducibility, the anti-thrombin activity of testing sample was (14.00 +/- 1.53) U/g and those of three different batch were (13.00 +/- 0.58) U/g, (17.00 +/- 1.15) U/g, (15.67 +/- 1.53) U/g respectively. CONCLUSION: The methods of TLC identification and anti-coagulant activity quantitatively could be used as a basis for improving the quality standard of Scolopendra subspinipes mutilans.

Automated multiple development thin-layer chromatography for separation of opiate alkaloids and derivatives.

There are three types of opiate alkaloids. First, the poppy alkaloids: morphine, codeine, thebaine, noscapine and papaverine; then, the semi-synthetic and synthetic derivatives used in therapy as antitussives and analgesics, such as pholcodine, ethylmorphine and dextromethorphan; at last narcotic compounds, diacetylmorphine (heroin) and opiates employed as substitutes in treatment of addiction: buprenorphine and methadone. For classical thin-layer chromatography (TLC) of opium alkaloids, it is necessary to use complex eluents with strong alkaline substances to obtain a clean separation between morphinan and isoquinoline compounds. This study purposes the planar chromatographic analysis of these substances by the automated multiple development (AMD) compared with results obtained by classical TLC method. The aim of this work was to achieve the best separation of these opiate alkaloids and derivatives by this modern technique of planar chromatography. The AMD system provided a clean separation for each of three opiates groups studied and the best results have been obtained with universal gradient: methanol 100, methanol-dichloromethane 50/50, dichloromethane 100, dichloromethane 100, hexane 100 for opium alkaloids and with gradient A: 5% of 28% ammonia in methanol 100, acetone 100, acetone 100, ethyl acetate-dichloromethane 50/50, dichloromethane 100 for antitussives and substitutes. Two reagents were used for the detection of alkaloids by spraying: Dragendorff and iodoplatinate reagents. The detection limits with these two reagents were 1 microg for ethylmorphine, thebaine, papaverine, codeine, and 2 microg for morphine and noscapine and other alkaloids.

[New method for selectivity optimization in thin layer chromatography and its application in pharmaceutical analysis].

A new experimental design method named the step climbing method (SCM), as well as a new global criterion (NRC), are proposed for the selectivity optimization of thin layer chromatography. The method offers chromatographers a convenient means to decide the optimum developer composition for thin layer chromatography. The principle of the method is described, and examples of applications in pharmaceutical analysis are given to certify the feasibility of the method. Clearly, it may also be used for the selectivity optimization in high performance liquid chromatography.

Chionanthus virginicus L.: phytochemical analysis and quality control of herbal drug and herbal preparations.

Root barks of Chionanthus virginicus L. are used in homeopathic medicines in the treatment of icterus and hepatitis. The objective of this study is to identify novel secoiridoids and lignans and to develop a simple and reliable HPLC method for the determination of oleuropein, phillyrin, total secoiridoids and total lignans for quality control and stability studies of C. virginicus herbal drug and preparations. Secoiridoids and lignans were purified by preparative HPLC. Compounds previously described were identified by HPLC according to their retention times and UV spectra. Structures of new compounds were determined by NMR. Two compounds namely excelside B and acetoxypinoresinol-4"-O-beta-D-glucoside are described for the first time in the drug. HPLC separation was performed on Symmetry C18 (Waters) by gradient elution using acetonitrile and 0.2% aqueous phosphoric acid. The method was validated for specificity, linearity, precision, accuracy, limits of detection and quantification for simultaneous determination of secoiridoids and lignans in herbal drug and herbal preparations as mother tinctures. The proposed HPLC method is linear in the range studied (r2 > or = 0.9989) for all the analytes. The method is precise with intra- and inter-day variations of less than 4%. The mean recoveries of the analytes range from 99.65 to 102.81%. The method is successfully applied to the quantification of nine compounds belonging to secoiridoids and lignans and for the stability studies of these compounds. The study allowed completing the phytochemical knowledge of C. virginicus. This simple developed assay could be used as tools for routine quality control of C. virginicus herbal drug and herbal medicinal products.

HPTLC method for the estimation of alkaloids of Cinchona officinalis stem bark and its marketed formulations.

We report a sensitive method for the estimation of quinine (Qn), cinchonine (Cn), and cinchonidine (Cnd) and a new method based on fluorescence enhancement and detection and quantification of quinidine (Qnd) from Cinchona stem bark and its formulations, using HPTLC. Standard solutions of Qn, Qnd, Cn, and Cnd were applied on precoated HPTLC plates and developed with chloroform/diethylamine (9.6:1.4 v/v). The plates were scanned and quantified at 226 nm for Qn, Cn, Cnd and for Qnd at 366 nm in fluorescence and reflectance mode ([symbol: see text] K400 filter). The method was validated for precision, accuracy and repeatability. Further, the stem bark of Cinchona officinalis and some herbal and homeopathic formulations were evaluated for their individual alkaloid content applying the developed method.

Control de calidad de la tintura homeopática de Capsicum annuum L / Control of quality of the homeopathic tincture of Capsicum annuum L

El propósito de este trabajo fue obtener la tintura de Capsicum annuum L. según el método de la escuela francesa, a un título de etanol del 90 por ciento y establecer sus índices de calidad tales como: características organolépticas, imagen capilar, índice de refracción, densidad relativa, pH, título etanólico y porcentaje de residuo seco. Se realizaron reacciones de identificación para detectar la presencia de carotenoides y determinar la prueba del vanadato. Por cromatografía en capa delgada fue estandarizado un perfil de la tintura. En todos los lotes obtenidos, sus índices de calidad se encontraron dentro de los límites establecidos por las farmacopeas tomadas como referencias. Se realizó un estudio para determinar el tiempo de vida útil de la tintura por 1 año a temperatura ambiente en frascos de vidrio de color ámbar de 30 mL y pudo comprobarse que en estas condiciones conservó óptimamente sus características. El conteo microbiano de la tintura se mantuvo por debajo de los niveles permisibles durante todo el experimento. Estos resultados demostraron que es realmente posible obtener esta tintura en Cuba con una calidad similar a la exigida por farmacopeas homeopáticas oficiales

Comparación entre el bromuro de pancuronio genérico y el Pavulon®1 / Comparison between generic pancuronium bromide and Pavulon®1

Históricamente se ha planteado el conflicto sobre la eficacia y la seguridad terapéutica entre marcas genéricas y la marca original, lo cual llevó a desarrollar el siguiente estudio. Objetivos: 1) realizar ensayos fisicoquímicos de ampollas que contenían 4 mg/2ml de bromuro de pancuronio, en una marca genérica (G) y en una original (P = Pavulon®), 2) determinar la eficacia y la seguridad terapéutica de ambas drogas, y 3) comparar los resultados entre ambas marcas, tomando como patrón de referencia la marca original. Materiales y métodos: Ensayos fisicoquímicos realizados conforme la Farmacopea Británica 2001 (FB). Eficacia y seguridad terapéutica evaluada mediante un estudio prospectivo, randomizado y doble ciego en cincuenta pacientes ASA I-II a quienes se administró 2 mcg/kg de citrato de fentanilo, 5 mg/kg de tiopental sódico cinco minutos después y 0.1 mg/kg de bromuro de pancuronio. La anestesia se mantuvo con sevoflurano 2 por ciento. Se evaluó el tiempo T1 para alcanzar los valores porcentuales 95,75,25,0 y 25 de recuperación o duración clínica. Comparación: Test de Mann - Whitney, p < 0.05. Resultados: Los ensayos fisicoquímicos para el grupo genérico y el Pavulon® cumplieron con las especificaciones de la FB. En el grupo genérico, los tiempos necesarios para que T1 disminuya hasta 95 y 75 por ciento resultaron respectivamente 33.15 y 48.36 segundos; para que disminuya al 25 por ciento y 0 por ciento, 1.50 Y 2.97 minutos, y la duración clínica fue de 108.99 minutos. En el grupo Pavulon®, el tiempo requerido para T1 = 95 Y 75 por ciento fue de 24.89 y 41.54 segundos respectivamente, mientras que para llegar al 25 y 0 por ciento fueron necesarios 1.34 y 2.71 minutos; la duración clínica en este grupo fue de 111.99 minutos. Conclusiones: Los tiempos evaluados no arrojaron diferencia estadística significativa entre ambas marcas.

Avaliação da atividade citotóxica, antiviral e antimicrobiana de Apocynaceae amazônicas / Evaluation of the activity cytotoxic, antiviral and antimicrobial of Apocynaceae Amazonian

A necessidade de se introduzir novos fármacos quimioterápicos é patente. Para tanto, a modelagem molecular, a terapia gênica e os produtos naturais têm sido os caminhos escolhidos para a obtenção de novas moléculas. As florestas brasileiras estão entre os principais celeiros de biodiversidade, grande parte não estudada do ponto de vista fitoquímico e farmacológico. Isso implica em grandes possibilidades de identificação de novos fármacos, uma vez que a riqueza da biodiversidade biológica pode ser refletida na riqueza da biodiversidade química. Trinta e oito extratos provenientes de espécies de Apocynaceae foram submetidos a um estudo de triagem farmacológica antiviral, antimicrobiana e citotoxicidade, in vitro...(AU)