Enhancement of fine structure of ultraviolet spectra applied to direct extraction of drugs from urine

Abstract

Basic drugs are extracted from urine or drug preparations at pH 9.5-11 into cyclohexane or heptane containing a small amount (ca. 0.1%) of benzene. The presence of the benzene introduces fine structure in the ultraviolet spectra of compounds that ordinarily give qualitatively similar spectra. This allows the fingerprint identification of the compounds. For example, amphetamine, ephedrine, and meperidine can be readily identified. A double-beam recording spectrophotometer is used to blank out the benzene absorption by placing the cyclohexane benzene or heptane-benzene solvent mixture in the reference path.

Detection of amphetamine in air by solid adsorbent preconcentration and gas chromatographic analysis

“…D-Amphetamine sulfate (BDH lot 30603-35403) was obtained from Health and Welfare Canada. The free base was extracted from the sulfate salt following the procedure described by Predmore (12). Tenax-GC (35-60 mesh) was obtained from Supelco Inc. (Bellefonte, PA), Ultra Bond PEGS (80-100 mesh) from Alltech Assoc.…”

Ultraviolet and light absorption spectrometry

“…Alizarine complexone [450; 0.5-6 ppm] 3,5-Dinitropyrocatechol, Brilliant Green (CC14) [625] Molybdogermanate, acetone [430] Hf l,5-Bis(2-hydroxyphenyl)-3-cyanoformazan [580; 9.3 X 10 l-(2-Pyridylazo)-2-naphthol [545; 3. 1-Phenyl-2,3-dimethylpyrazalone-5-azo-4-pyrogallol [460; 0.46-4.6 ppm]…”

“…with NaBH" in MeOH [246] Benzidine Oxidn. with Mn(P04)23", Mn2(S04)3 [425; 6.18 X 104] Benzoic acid and o-, Fe(III) [300,260,225,525] mp-hydroxy [580] Carbonyl compounds 2,4-Dinitrophenylhydrazine (rz-C7Hle-CCl4) [430] Carboxylic acids HONH34, carbodiimide coupling reag., Fe(III) salt Carboxylic acids, Safranine T, acridine yellow, methylene blue (CHC13) arom.…”

“…Tetraphenylborate has been determined using a replacement reaction with solid mercuric chloranilate (320). The addition of 0.1% benzene to heptane or cyclohexane used for extraction of drugs from urine or pharmaceutical preparations greatly enhances the ultraviolet fine structure and allows better identification of specific drugs (430). A simplex optimization procedure applied to the chromotropic acid method for formaldehyde has shown that the order of reagent addition is important (379).…”

“…aq. HC1) [650] 7 Arsenazo III, Zephiramine (CHC13) [655; 6.2 104] p-Carboxyphenylazochromotropic acid [595; 1.13 104] Chromazurol S, quaternary ammonium salts [625; 0.09-2.29 ppm] Cyelopentanone-2-carboxyanilide (i-BuCOMe) [360; 10-60 ppm] Hydroxynapthol blue [530; 4.1 X 103] Malachite Green, benzoate (PhCl) [635; 8.3 X 104] 2-Mercaptopyridine-l-oxide (Bu3P04) [490] 4-(2-Pyridylazo)naphthol (trioctylphosphine oxide) [530] 1-(4-Tolyl)-2-methyl-3-hydroxy-4-pyridone (CHC13) [319; 3.1 X 104] iV-p-Tolyl-o-methoxybenzohydroxamic acid (CHC13) [360; 2.1 X 103] Zephiramine, KSCN (CHC13) [305; 1.5 X 104]iV-p-Chlorophenyl-p-methoxybenzohydroxamic acid (CHC13)[545; 0.5-15 ppm] /V-(p-fV,iV-Dimethylanilino-3-methoxy-2-naphtho)hydroxamic acid (CHC13) [570; 1.2 X 104] Ferron, dithionite (tribenzylamine in CHC13)[430] 631 8-Hydroxyquinoline, dithionite (CC14)[420] 632 8-Hydroxy quino line, HC104 (PhN02) [640; 6.02 X 103J N-o-Methoxyphenyl-2-thenohydroxamic acid (CHC13) 545; -5-dimethylaminophenol [410; 1.4 104] l-Phenylazo-2-hydroxy-3-naphthylhydroxamic acid (C6H6)[545; 6.54 X 104] l-Phenyl-2-methyl-3-hydroxy-4-pyridone (CHC13)[497, 625; 4.1 X 103, 5.6 X 103]…”