RESUMO
The case histories are presented of three separate incidents of poisoning by ingestion of Hemlock Water Dropwort tubers (Oenanthe crocata). Two of these cases involved a fatality. An analytical profile is provided for oenanthotoxin, the major toxic principal of the tubers. Chromatographic, spectroscopic and mass spectral data for related compounds are also given.
Assuntos
Álcoois Graxos/análise , Intoxicação por Plantas/metabolismo , Adulto , Alcinos , Cromatografia Líquida de Alta Pressão , Cromatografia em Camada Fina , Enedi-Inos , Feminino , Humanos , Masculino , Espectrometria de Massas , Extratos Vegetais/análise , Espectrofotometria UltravioletaRESUMO
A scheme of analysis is described in which the particular advantages of high-performance liquid chromatography (HPLC), fluorescence spectroscopy and radioimmunoassay (RIA) are exploited to the greatest effect. RIA affords a rapid and sensitive preliminary screening method, while the subsequent HPLC analysis using fluorimetric detection yields quantitative chromatographic evidence together with characteristic fluorescence spectra. Fractionation of samples by HPLC followed by RIA of the fractions gives further confirmation of the presence of LSD and its metabolites. The combined methodology has been applied to the analysis of LSD in body fluids for forensic and clinical purposes. Levels down to 0.5 ng of LSD per ml can be detected using the minimum of sample.
Assuntos
Dietilamida do Ácido Lisérgico/análise , Cromatografia Líquida de Alta Pressão , Feminino , Humanos , Dietilamida do Ácido Lisérgico/sangue , Dietilamida do Ácido Lisérgico/urina , Masculino , Radioimunoensaio , Espectrometria de Fluorescência , Estômago/análiseRESUMO
A novel technique of on-line photochemical derivatization is described which can enhance considerably both the sensitivity and specificity of detection in high-performance liquid chromatography (HPLC).. Material eluting from the column is irradiated with a high flux of UV light, which may induce a reaction to form fluorescent or highly UV-absorbing products. The irradiated eluent then passes into a suitable detector. The photochemical reactor as a neglible effect on resolution, and reaction is achieved in 1-5 sec. An example of the use of this technique is in the detection of cannabinol CBN), a component of cannabis, which is converted into a highly fluorescent compound on irradiation with UV light. Thus, if a sample containing CBN is chromatographed and the column eluent irradiated, CBN can be detected (as the fluorescent photoproduct) with a sensitivity of less than 1 ng. If the chromatogram is then repeated without UV irradiation, only naturally fluorescent products are detected. A compairson of the two chromatograms allows these to be eliminated and leads to a very high specificity for the method. This approach is being developed as the basis of a rapid, sensitive and specific method for the detection of cannabinoids in body fluids. It is expected, however, that photochemical derivatization will extend the use of HPLC to many substances that cannot be satisfactorily detected at present.
Assuntos
Canabinoides/urina , Cromatografia Líquida de Alta Pressão/métodos , Humanos , Fotoquímica , Espectrometria de FluorescênciaRESUMO
A simple, rapid and sensitive method is described for the analysis of unchanged benzodiazepine drugs and their metabolites, in human and animal tissues, using the proteolytic enzyme subtilisin Carlsberg followed by reverse-phase liquid chromatography. The enzymic digestion yields far higher recoveries than conventional extraction methods, while the liquid chromatogrpahic analysis allows the rapid separation and detection of nanogram quantities of these drugs without the need for elaborate "clean-up" procedures.
Assuntos
Benzodiazepinas/análise , Animais , Benzodiazepinas/intoxicação , Cromatografia Líquida de Alta Pressão , Cobaias , Humanos , Fígado/análise , Métodos , SubtilisinasRESUMO
A microparticulate cation-exchange column has been evaluated for the chromatography of thirty compounds selected as representative of a wide variety of drug substances. Although the column exhibited a strong partition effect besides the expected ion-exchange mechanism, the retention of drugs could be predictably influenced by variation of the eluent ionic strength and organic solvent content. For acidic drugs the column showed little selectivity (although a salting-out effect increased retention at high eluent ionic strengths), but for basic substances Partisil SCX may afford a useful separative medium offering reasonable chromatographic efficiency (HETP is approximately 0.1 mm). The column longevity, however, is at present questionable.
Assuntos
Resinas de Troca de Cátion , Cromatografia Líquida de Alta Pressão , Resinas de Troca Iônica , Preparações Farmacêuticas/análise , Cromatografia por Troca Iônica , Estudos de Avaliação como Assunto , Concentração de Íons de Hidrogênio , Lipídeos/análise , Métodos , Microquímica , Polarografia , SolventesRESUMO
The performance of a commonly used high-pressure liquid chromatographic stationary phase, octadecylsilane, has been evaluated for 30 compounds selected as representative of a wide variety of drug substances. Chromatographic behavior is found to be highly predictable on the basis of pKa and partition coefficient, and the stationary phase should be especially valuable for the separation of acidic and neutral drugs. For basic drugs, however, the column efficiency is poor, detracting from the overall usefulness.
