Abstract
An investigation was carried out on the isolation of 28 drugs from blood by column chromatography on Amberlite XAD-2. The following substances were added to postmortem blood specimens at concentrations generally of 1–10 μg/ml: barbital, heptabarbital, hexobarbital, pentobarbital, phenobarbital, phenylbutazone, monocrotophos, amidopyrine, carbromal, diazepam, meprobamate, methaqualone, nitrazepam, phenazetin, chlorpromazine, dibenzepin, diphenhydramine, haloperidol, imipramine, mescaline, methadone, morphine, pentazocine, pethidine, tilidine, triflupromazine, verapamil, N-propylajmalinium bitartrate. The samples were purified by column chromatography on Amberlite XAD-2 and simple solvent extraction and subsequently quantitated by gas chromatography. By systematic variation of the conditions for adsorption of the drugs and desorption from the resin, revoveries of more than 80% after XAD-2 column chromatography could be achieved for most drugs. Thereby it was demonstrated, that in cases of fatal poisoning or emergencies this procedure is a valuable tool for forensic and clinical toxicologists who have to find out the toxic agent by chemical analysis of the blood.
Zusammenfassung
Es wurden Untersuchungen über die säulenchromatographische Isolierung von 28 Arzneistoffen aus Blut an Amberlite XAD-2 durchgeführt. Die folgenden Substanzen wurden Leichenblutproben in Konzentrationen im allgemeinen von 1–10 μg/ml zugesetzt: Barbital, Heptabarbital, Hexobarbital, Pentobarbital, Phenobarbital, Phenylbutazon, Monocrotophos, Amidopyrin, Carbromal, Diazepam, Meprobamat, Methaqualon, Nitrazepam, Phenacetin, Chlorpromazin, Dibenzepin, Diphenhydramin, Haloperidol, Imipramin, Meskalin, Methadon, Morphin, Pentazocin, Pethidin, Tilidin, Triflupromazin, Verapamil, N-Propylajmalinium Bitartrat. Die Blutproben wurden säulenchromatographisch an Amberlite XAD-2 und durch eine einfache Lösungsmittelverteilung gereinigt, und anschließend wurden die Arzneimittel durch Gaschromatographie quantitativ bestimmt. Durch systematische Optimierung der Bedingungen für die Adsorption und die Desorption vom Kunstharz konnten für die meisten Substanzen Wiederfindungen von mehr als 80% nach XAD-2 Säulenchromatographie erreicht werden. Dieses Verfahren ist also ein wertvolles Hilfsmittel für den forensischen und klinischen Toxikologen, der bei tödlichen oder akut lebensbedrohlichen Vergiftungsfällen das wirksame Agens durch die Untersuchung des Blutes nachweisen muß.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Bastos, M. L., Jukofsky, D., Mulé, S. J.: Routine identification of drugs of abuse in human urine. III. Differential elution of the XAD-2 resin. J. Chromatogr. 81, 93–98 (1973)
Bastos, M. L., Jukofsky, D., Saffer, E., Chedekel, M., Mulé, S. J.: Modifications of the XAD-2 resin column method for the extraction of drugs of abuse from human urine. J. Chromatogr. 71, 549–553 (1972)
Bradlow, H. L.: Extraction of steroid conjugates with neutral resin. Steroids 11, 265–272 (1968)
Delbeke, F. T., Debackere, M.: Detection of sympathomimetic central nervous stimulants with special reference to doping. I. Comparative study of a conventional extraction procedure and adsorption chromatography using XAD-2 resin. J. Chromatogr. 133, 214–217 (1977)
Dupeyron, J. P., Bonnet, E., Lassechere, M., Fabiani, P.: Recherche des substance toxicomanogènes dans l'urine par chromatographie sur résine Amberlite XAD-2. I. Analgesique centraux. Ann. Fals. exp. Chim. 67, 451–462 (1974)
Dupeyron, J. P., Quattrocchi, F., Fabiani, P.: Recherche et dosage de toxiques dans le sang et l'urine par chromatographie sur résine d'Amberlite XAD-2. II. Dérivés terpéniques volatils. Ann. Fals. exp. Chim. 69, 229–246 (1976)
Fujimoto, J. M., Wang, R. I. H.: A method of identifying narcotic analgesics in human urine after therapeutic doses. Toxicol. appl. Pharmacol. 16, 186–193 (1970)
Gelbke, H. P., Schlicht, H. J.: Fatal poisoning with a plant protective containing monocrotophos, dodine, and dinocap. Europ. J. Toxicol. (in press) (1977a)
Gelbke, H. P., Schlicht, H. J.: Suicide by an overdosage of N-propylajmalinium bitartrate. Arch. Toxicol. 37, 135–141 (1977b)
Gelbke, H. P., Schlicht, H. J., Schmidt, G.: Fatal poisoning with verapamil. Arch. Toxicol. 37, 89–94 (1977)
Hetland, L. B., Knowlton, D. A., Couri, D.: A method for the detection of drugs at therapeutic dosages in human urine using adsorption column chromatography and thin-layer chromatography. Clin. chim. Acta 36, 473–478 (1972)
Ibrahim, G., Andryauskas, S., Bastos, M. L.: Application of Amberlite XAD-2 resin for general toxicological analysis. J. Chromatogr. 108, 107–116 (1975)
Kullberg, M. P., Gorodetzky, C. W.: Studies on the use of XAD-2 resin for detection of abused drugs in urine. Clin. Chem. 20, 177–183 (1974)
Kullberg, M. P., Miller, W. L., McGowan, F. J., Doctor, B. P.: Studies on the single extraction of amphetamine and phenobarbital from urine using XAD-2 resin. Biochem. Med. 7, 323–335 (1973)
Machata, G., Vycudilik, W.: Adsorptionsverfahren zur Bestimmung von Arzneimitteln in biologischem Material. Z. Rechtsmedizin 74, 43–46 (1974)
Machata, G., Vycudilik, W.: Isolierung von Drogen aus Blut mit makroretikulären Adsorberharzen. Arch. Toxicol. 33, 115–122 (1975)
Miller, W. L., Kullberg, M. P., Banning, M. E., Brown, L. D., Doctor, B. P.: Studies on the quantitative extraction of morphine from urine using nonionic XAD-2 resin. Biochem. Med. 7, 145–158 (1973)
Missen, A. W.: Procedures compared for extracting benzodiazepines from blood. Clin. Chem. 22, 927–928 (1976)
Missen, A. W., Lewin, J. F.: A non-ionic resin extraction of drugs in blood. Clin. chim. Acta 53, 389–390 (1974)
Mulé, S. J., Bastos, M. L., Jukofsky, D., Saffer, E.: Routine identification of drugs of abuse in human urine. II. Development and application of the XAD-2 resin column method. J. Chromatogr. 63, 289–301 (1971)
Pietrzy, D. J., Chu, C. H.: Amberlite XAD copolymers in reversed phase gravity flow and high pressure liquid chromatography. Anal. Chem. 49, 757–764 (1977)
Pranitis, P. A. F., Stolman, A.: The differential elution of drugs from XAD-2 resin. J. forens. Sci. 20, 726–730 (1975)
Pranitis, P. A. F., Milzoff, J. R. Stolman, A.: Extraction of drugs from biofluids and tissues with XAD-2 resin. J. forens. Sci. 19, 917–926 (1974)
Roerig, D. L., Lewland, D., Mueller, M., Wang, J. I. H.: Methods of identification and confirmation of abusive drugs in human urine. J. Chromatogr. 110, 349–359 (1975)
Sawada, H., Hara, A., Asano, S., Matsumoto, Y.: Isolation and identification of benzodiazepine drugs and their metabolites in urine by use of Amberlite XAD-2 resin and thin-layer chromatography. Clin. Chem. 22, 1596–1603 (1976)
Stolman, A., Pranitis, P. A. F.: XAD-2 resin drug extraction methods for biological samples. Clin. Toxicol. 10, 49–60 (1977)
Vycudilik, W.: Isolation of drugs with macroreticular resins. Determination of phentermine in blood. J. Chromatogr. 111, 439–442 (1975)
Wang, R. I. H., Mueller, M. A.: Identification of barbiturates in urine. J. pharm. Sci. 62, 2047–2049 (1973)
Weissman, N., Lowe, M. L., Beattie, J. M., Demetriou, J. A.: Screening method for detection of drugs of abuse in human urine. Clin. Chem. 17, 875–881 (1971)
Wislocki, A., Martel, P., Ito, R., Dunn, W. S., McGuire, C. D.: A method for the detection of drugs of abuse in urine. Hlth Lab. Sci. 11, 13 (1974)
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Gelbke, H.P., Grell, T.H. & Schmidt, G. Isolation of drugs from blood by column chromatography on amberlite XAD-2. Arch Toxicol 39, 211–217 (1978). https://doi.org/10.1007/BF00368229
Received:
Issue Date:
DOI: https://doi.org/10.1007/BF00368229