Summary
The extraction of drugs from small blood samples (1 ml or less) for subsequent quantitative determination is described. Isolation was carried out by adsorption of the drugs to Amberlite XAD-2 resin utilizing a batch procedure that enabled the simultaneous extraction of up to 200 samples in approx. 5 hours. A new desorption technique yielded extracts of high purity that could be used directly for gas chromatographic or radioimmunological determinations, even if hemolyzed or putrid blood was to be examined. The following 26 substances were quantitated after addition to postmortem blood specimens at concentrations of 1–10 μg/ml: tilidine, diphenhydramine, dibenzepine, imipramine, chlorpromazine, amphetamine, pentazocine, phenacetin, methaqualone, meprobamate, parathion, diazepam, digoxin, β-methyldigoxin, carbromal, glutethimide, amobarbital, pentobarbital, cyclobarbital, phenobarbital, diphenylhydantoin, carbutamide, tolbutamide, glycodiazin, tolazamide and chlorpropamide. Thereby recoveries of 60–100% could be achieved. The reproducibility of the procedure was satisfactory as demonstrated by coefficients of variation of 3.7–8%.
Zusammenfassung
Es wird die Extraktion von Arzneistoffen aus kleinen Blutproben (1 ml oder weniger) für die nachfolgende quantitative Bestimmung beschrieben. Die Isolierung der Substanzen erfolgte durch Adsorption an ein Kunstharz (Amberlite XAD-2) mittels eines Batch-Verfahrens, das die Aufarbeitung von bis zu 200 Proben in ungefähr 5 Stunden ermöglichte. Die Anwendung einer neuartigen Desorptionstechnik führte selbst bei zersetzten Blutproben zu sehr sauberen Extrakten, die direkt für gaschromatographische oder radioimmunologische Bestimmungen verwendet werden konnten. Nach Zusatz zu Leichenblut in Konzentrationen von 1–10 μg/ml wurden die folgenden 26 Wirkstoffe quantitativ bestimmt: Tilidin, Diphenhydramin, Dibenzepin, Imipramin, Chlorpromazin, Amphetamin, Pentazocin, Phenacetin, Methaqualon, Meprobamat, Parathion, Diazepam, Digoxin, β-Methyldigoxin, Carbromal, Glutethimid, Amobarbital, Pentobarbital, Cyclobarbital, Phenobarbital, Diphenylhydantoin, Carbutamid, Tolbutamid, Glycodiazin, Tolazamid und Chlorpropamid. Dabei konnten Wiederfindungen von 60–100% erreicht werden. Die Reproduzierbarkeit war bei Variationskoeffizienten von 3,7–8% zufriedenstellend.
Similar content being viewed by others
References
Garriot, J. C., Di Maio, V. J. M., Zumwalt, R. E., Petty, C. S.: Incidence of drugs and alcohol in fatally injured motor vehicle drivers. J. forens. Sci. 22, 283–389 (1977)
Missen, A. W., Lewin, J. F.: Non-ionic resin extraction of drugs in blood. Clin. Chim. Acta 53, 389–390 (1974)
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)
Ibrahim, G., Andryauskas, S., Bastos, M. L.: Application of Amberlite XAD-2 resin for general toxicological analysis. J. Chromatog. 108, 107–116 (1975)
Machata, G., Vycudilik, W.: Isolierung von Drogen aus Blut mit makroretikulären Adsorberharzen. Arch. Toxicol. 33, 115–122 (1975)
Pranitis, P. A. F., Stolman, A.: The differential elution of drugs from XAD-2 resin. J. forens. Sci. 20, 726–730 (1975)
Vycudilik, W.: Isolation of drugs with macroreticular resins. Determination of Phentermine in blood. J. Chromatog. 111, 439–442 (1975)
Dupeyron, J. P., Quattroccki, F., Fabiani, P.: Recherche et dosage de toxiques dans le sang et l'urine par chromatographie sur résine d'Amberlite XAD-2. Dérivés terpéniques volatils. Ann. Fals. Exp. Chim. 69, 229–246 (1976)
Missen, A. W.: Procedures compared for extracting benzodiazepines from blood. Clin. Chem. 22, 927–928 (1976)
Gelbke, H. P., Grell, T. H., Schmidt, Gg.: Isolation of Drugs from Blood by column chromatography on Amberlite XAD-2. Arch. Toxicol. (In press)
Braselton, W. E., Ashline, H. C., Bransome, E. D.: Formation of thermally stable derivatives for determination of Tolbutamide and Chlorpropamide by gas chromatography. Anal. Letters 8, 301–313 (1975)
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. Chromatog. 71, 549–553 (1972)
Kullberg, M. P., Miller, W. L., McGowan, F. J., Doctor, E. P.: Studies on the single extraction of amphetamine and phenobarbital from urine using XAD-2 resin. Biochem. Med. 7, 323–335 (1973)
Miller, W. L., Kullberg, M. P., Banning, M. E., Brown, L. D., Doctor, E. P.: Studies on the quantitative extraction of morphine from urine using nonionic XAD-2 resin. Biochem. Med. 7, 145–158 (1973)
Roerig, D. L., Lewand, D., Mueller, M., Wang, R. I. H.: Methods of identification and confirmation of abusive drugs in human urine. J. Chromatog. 110, 349–359 (1975)
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. Chromatog. 133, 214–217 (1977)
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)
Gelbke, H. P., Schlicht, H. J., Schmidt, Gg.: Radioimmunological screening and gas chromatographic identification of diazepam in blood and serum. Arch. Toxicol. 38, 295–305 (1977)
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Schlicht, H.J., Gelbke, H.P. A micromethod for the isolation of drugs from blood using Amberlite XAD-2. Z Rechtsmed 81, 25–30 (1978). https://doi.org/10.1007/BF00200596
Received:
Issue Date:
DOI: https://doi.org/10.1007/BF00200596