| Autor: |
S.J. Mulé, D. Jukofsky, M.L. Bastos |
| Rok vydání: |
1973 |
| Předmět: |
|
| Zdroj: |
Journal of Chromatography A. 81:93-98 |
| ISSN: |
0021-9673 |
| DOI: |
10.1016/s0021-9673(01)82320-7 |
| Popis: |
The differential elution of the XAD-2 resin consisted of a sequential solvent extraction of drugs from the resin as follows: after passing the urine over the resin, the columns were transferred to centrifuge tubes containing 0.1 N hydrochloric acid and eluted with 10 ml of isopropyl ether. The tubes were thoroughly shaken and the phases were separated by freezing the aqueous layer pouring off the isopropy. ether. This phase was evaporated to dryness and the residues containing primarily the acidic and neutral drugs were applied to Polygram silica gel sheets and developed in chloroform-methanol-ammonia (90:10:1). The XAD-2 resin columns saved for the second elution were placed on the original centrifuge tubes containing the frozen acidic aqueous phase. The resins were eluted with two 10-ml portions of chloroformisopropanol (3:1). One millilitre of 0.125 M borax solution was added to each tube (pH 8–9.5), it was shaken and the phases were separated. The organic phases were evaporated to dryness and the residues containing primarily the basic and some neutral drugs were applied to silica gel thin-layer plates and developed in ethyl acetate-methanol-water-ammonia (85:10:3:1). The acidic, basic, and neutral drugs were detected by sequential chromogenic spraying of the chromatographic sheets and plates. Total recovery of the barbiturates was about 81% and for the basic drugs, it ranged from about 80 to 100%. The percentage increase in drugs detected with the differential elution technique as compared to the single elution method ranged from 2.4 to 100%. A decrease was observed only with d-propoxyph50%) and phenylpropanolamine (6.2%). |
| Databáze: |
OpenAIRE |
| Externí odkaz: |
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