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6.
J Chromatogr Sci ; 44(9): 557-60, 2006 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-17059683

RESUMO

A sensitive and reproducible reversed-phase high-performance liquid chromatography (HPLC) method using photodiode array detection is established for the simultaneous quantitation of important root alkaloids of Rauvolfia serpentina, namely, reserpine, ajmaline, and ajmalicine. A Chromolith Performance RP-18e column (100 x 4.6-mm i.d.) and a binary gradient mobile phase composed of 0.01 M (pH 3.5) phosphate buffer (NaH(2)PO(4)) containing 0.5% glacial acetic acid and acetonitrile are used. Analysis is run at a flow rate of 1.0 mL/min with the detector operated at a wavelength of 254 nm. The calibration curves are linear over a concentration range of 1-20 microg/mL (r = 1.000) for all the alkaloids. The various other aspects of analysis (i.e., peak purity, similarity, recovery, and repeatability) are also validated. For the three components, the recoveries are found to be 98.27%, 97.03%, and 98.38%, respectively. The limits of detection are 6, 4, and 8 microg/mL for ajmaline, ajmalicine, and reserpine, respectively, and the limits of quantitation are 19, 12, and 23 microg/mL for ajmaline, ajmalicine, and reserpine, respectively. The developed method is simple, reproducible, and easy to operate. It is useful for the evaluation of R. serpentina.


Assuntos
Ajmalina/análise , Cromatografia Líquida de Alta Pressão/métodos , Rauwolfia/química , Reserpina/análise , Alcaloides de Triptamina e Secologanina/análise , Calibragem , Padrões de Referência , Reprodutibilidade dos Testes
7.
J Chromatogr B Biomed Appl ; 661(1): 47-53, 1994 Nov 04.
Artigo em Inglês | MEDLINE | ID: mdl-7866551

RESUMO

After ingestion of an unknown dose of detajmium, a 14-year-old female collapsed with asystolia. Resuscitation efforts were not successful. A medicolegal autopsy was carried out, and blood, liver and gastric content were extracted and analyzed by gas chromatography-mass spectrometry (GC-MS). After derivatization with acetic anhydride, detajmium and twelve of its derivatives and metabolites were identified. The main metabolic pathways include hydroxylation and subsequent O-methylation of the indol ring, and oxidation as well as reduction of the C-21 hydroxyl function. Cleavage of the N-alkyl side-chain is a further, possibly non-enzymatic degradation pathway. Artifact formation induced by acetylation included dehydratation of the hydroxyl function of C-21 and the N-alkyl side-chain. The detajmium concentration in blood of the decreased was determined by high-performance liquid chromatography with fluorimetric detection (12 micrograms/ml).


Assuntos
Ajmalina/análogos & derivados , Antiarrítmicos/intoxicação , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Conteúdo Gastrointestinal/química , Fígado/química , Anidridos Acéticos/análise , Adolescente , Ajmalina/análise , Ajmalina/sangue , Ajmalina/intoxicação , Antiarrítmicos/análise , Antiarrítmicos/sangue , Autopsia , Feminino , Humanos
8.
Ther Drug Monit ; 14(5): 391-6, 1992 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-1448847

RESUMO

Lorajmine is a monochloroacetyl derivative of ajmaline with electrophysiological properties somewhat different from those of the compound of origin. Since lorajmine is rapidly hydrolyzed to ajmaline by plasma and tissue esterases, it is crucial to measure plasma levels of both drugs separately. A major problem in assaying lorajmine is its chemical instability in plasma both after blood sampling and during the extraction procedure. Furthermore, lorajmine (unlike ajmaline) is not fluorescent and has a very low UV absorbance, so the standard detectors for high-performance liquid chromatography cannot be used. We describe a new method that solves the problems of instability and sensitivity. Plasma esterases are first blocked pharmacologically (neostigmine); ajmaline is then measured by direct on-column injection of samples. Last, lorajmine is completely converted to ajmaline, extracted, and measured with a fluorescence detector. The molar concentration of ajmaline obtained in the last step, minus that found by direct injection, gives the concentration of lorajmine. Some examples of pharmacokinetic applications are also given.


Assuntos
Ajmalina/análise , Administração Oral , Adulto , Ajmalina/farmacocinética , Nó Atrioventricular/efeitos dos fármacos , Disponibilidade Biológica , Cromatografia Líquida de Alta Pressão/métodos , Esterases/antagonistas & inibidores , Esterases/sangue , Fluorometria , Sistema de Condução Cardíaco/efeitos dos fármacos , Humanos , Concentração de Íons de Hidrogênio , Injeções Intravenosas , Masculino , Pessoa de Meia-Idade , Função Ventricular/efeitos dos fármacos
9.
J Forensic Sci ; 33(2): 558-61, 1988 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-3373173

RESUMO

An infant fatality following accidental ingestion of ajmaline is described. Ajmaline was determined by thin-layer chromatography and infrared spectrophotometry, and quantitated by high performance liquid chromatography. The ajmaline concentration in blood was 5.5 micrograms/mL. The toxicological data relevant to the interpretation of case findings are presented.


Assuntos
Ajmalina/intoxicação , Ajmalina/análise , Química Encefálica , Pré-Escolar , Cromatografia Líquida de Alta Pressão , Cromatografia em Camada Fina , Feminino , Conteúdo Gastrointestinal/análise , Humanos , Fígado/análise , Espectrofotometria Infravermelho
12.
Z Rechtsmed ; 82(3): 231-6, 1978 Dec 20.
Artigo em Alemão | MEDLINE | ID: mdl-742214

RESUMO

A case of N-Propylajmalinum bitartrate intoxication (Neo-Gilurytmal) is reported in which the death occurred within 20 minutes after the consumption of the drug. The quantitative estimation of the drug after isolation using Extrelut--columns was carried out in stomach spectrometrically, in the blood, bile, liver, kidney, and brain by gaschromatography after trifluoroacetylation. A high Prajmalium-bitartrate concentration was found in the blood (3,85 mg/l), negative results in bile and brain, low levels in liver (0,29 mg/kg wet weight) and kidney (0,06 mg/kg wet weight). Prajmalium-bitartrate was ingested together with beer, and a blood alcohol concentration of 0.061% was determined. Furthermore, a quantity corresponding to six tablets of Neo-Gilurytmal was still found in the stomach. The rapid fatal progress of the intoxication is explained as a strong effect of the drug on the heart due to the alcohol accelerated resorption of the substance.


Assuntos
Ajmalina/análogos & derivados , Adulto , Ajmalina/análise , Ajmalina/intoxicação , Bile/análise , Química Encefálica , Cromatografia Gasosa , Sinergismo Farmacológico , Etanol/metabolismo , Feminino , Humanos , Rim/análise , Fígado/análise , Fatores de Tempo
14.
Arch Toxicol ; 37(2): 135-41, 1977 Jun 18.
Artigo em Inglês | MEDLINE | ID: mdl-577683

RESUMO

The toxicological findings after suicidal poisoning with N-propylajmalinium bitartrate (NPAB) are presented. For isolation of NPAB the biological material was homogenized and the drug was isolated by adsorption on Amberlite XAD-2. After column chromatographic purification on Sephadex LH-20 quantitative determinations were carried out by gas chromatography of the trifluoroacetate. The identity of the material finally obtained was checked by various chromatographic and spectrometric methods. The following concentrations of NPAB were found: liver 58 microgram/g, kidney 32 microgram/g, brain 16 microgram/g, muscle less than 10 microgram/g, heart less than 5 microgram/g, blood less than 5 microgram/g, gastric contents 600 mg (total). 1200 mg of NPAB had been swallowed; thus the amount of NPAB, that had crossed into blood, was approx. 500-600 mg corresponding to a dose of 9-11 mg/kg body weight.


Assuntos
Ajmalina/análogos & derivados , Adulto , Ajmalina/análise , Ajmalina/intoxicação , Cromatografia Gasosa , Cromatografia em Gel , Cromatografia por Troca Iônica , Feminino , Humanos , Métodos , Compostos de Amônio Quaternário/intoxicação , Suicídio
16.
J Pharm Sci ; 64(2): 341-2, 1975 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-1127594

RESUMO

Herbadine, a novel dihydroindole alkaloid, was isolated from the arterial parts of Vinca libanotica Zucc. (Apocynaceae). The physical and spectral data (UV, IR, NMR, and mass spectroscopy) indicated the alkaloid to be a derivative of aimaline. Comparative high-resolution NMR studies with quebrachidine and high-resolution mass spectral studies established the structure of the alkaloid to be 2-epi-3-hydroxyquebrachidine. Herbadine was previously isolated from another species by Russian workers and a structure was postulated. The current paper gives evidence for a corrected structure of herbadine.


Assuntos
Ajmalina/análogos & derivados , Alcaloides de Vinca/análise , Ajmalina/análise , Indóis/análise , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Espectrofotometria Infravermelho , Espectrofotometria Ultravioleta
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