Doxazosin

Molecular formula: C23H25N5O5 Molecular weight: 451.5 CAS Registry No.: 74191 -85-8 (doxazosin), 77883-43-3 (doxazosin mesylate)

SAMPLE

Matrix: blood Sample preparation: Condition a Bond Elut C18 SPE cartridge with 1 mL MeOH and 1 mL water. 1 mL Plasma + 50 |JLL 1 |xg/mL propranolol in MeOH + 250 |JLL MeOH, agitate briefly, let stand for 10 min, centrifuge at 3000 g for 10 min. Add the supernatant to the SPE cartridge, wash with 1 mL MeOH: water 30:70, wash with 1 mL water, elute with 1 mL MeOH.acetic acid 99.5:0.5. Evaporate the eluate to dryness under a stream of air, reconstitute the residue in 150 |xL mobile phase, inject an aliquot.
HPLCVARIABLES

Column: 150 X 4.6 5 |xm Zorbax CN Mobile phase: MeOH: buffer 50:50 (Buffer was 10 mM perchloric acid and 1.8 mM sodium heptanesulfonate.) Flow rate: 1 Detector: F ex 245 em bandpass 320-390 (Corning 7-60 filter)
CHROMATOGRAM

Retention time: 5 Internal standard: propranolol (3.5) Limit of detection: 1 ng/mL

KEYWORDS

plasma; pharmacokinetics; SPE

REFERENCE
Jackman, G.P.; Colagrande, F.; Louis, W.J. Validation of a solid-phase extraction high-performance liquid chromatographic assay for doxazosin. J.Chromatogr., 1991, 566, 234-238

SAMPLE

Matrix: blood Sample preparation: 250 |xL Serum + 250 jxL 20 ng/mL prazosin in MeOH: water 30:70, vortex for 30 s, add 1.5 mL ethyl acetate, vortex for 15 s, centrifuge at 3000 rpm for 2 min. Remove the organic layer and evaporate it to dryness in a vortex evaporator at 40 for 10 min, reconstitute the residue in 200 jxL MeOH-.water 50:50, inject a 50 \xL aliquot.
HPLCVARIABLES

Guard column: 50 X 3.9 40 jim glass beads Column: 150 X 4.6 alumina-based reversed-phase gamma RP-I (ES Industries) Mobile phase: MeCN: MeOH: 25 mM pH 10.9 sodium carbonate 15:15:70 (At the end of each day flush with about 75 mL MeOH .water 50:50 until pH of effluent is neutral.) Flow rate: 2 Injection volume: 50 Detector: F ex 246 em 389 (cutoff filter)
CHROMATOGRAM Retention time: 4.9

Internal standard: prazosin (1.8) Limit of quantitation: 0.5 ng/mL KEYWORDS serum REFERENCE
Fouda, H.G.; Twomey, T.M.; Schneider, R.R Liquid chromatographic analysis of doxazosin in human serum with manual and robotic sample preparation. J.Chromatogr.Sci., 1988, 26, 570-573

SAMPLE Matrix: blood Sample preparation: 1 mL Whole blood + 5 mL diethyl ether, shake for 10 min, centrifuge at 2000 rpm for 5 min, freeze in acetone/dry ice. Remove the organic layer and add it to 100 |JLL 50 mM sulfuric acid, shake for 10 min, centrifuge at 2000 rpm for 5 min, inject a 20 |xL aliquot of the aqueous layer. HPLCVARIABLES Column: 250 X 4 5 |jim Spherisorb ODS Mobile phase: MeOH: water 55:45 containing 10 mM pentane sodium sulfate and 9 mM tetramethylammonium chloride, adjusted to pH 3.4 with glacial acetic acid Flow rate: 1.8 Injection volume: 20 Detector: F ex 254 em 400 (cut-off filter) CHROMATOGRAM Retention time: 9 Internal standard: doxazosin OTHER SUBSTANCES Extracted: trimazosin KEYWORDS whole blood; doxazosin is IS REFERENCE
Hughes, M.A.; Meredith, RA.; Elliott, H.L. The determination of trimazosin and its metabolite CP23445 in whole blood by high performance liquid chromatography using fluorescence detection. J.Pharmacol.Methods, 1984, 12, 29-34

SAMPLE Matrix: solutions HPLCVARIABLES Column: 150 X 4.6 12 |xm l-myristoyl-2-[(13-carboxyl)-tridecoyl]-sn-3-glycerophosphocholine chemically bonded to silica (Regis) Mobile phase: MeCN: 100 mM pH 7.0 phosphate buffer 20:80 Flow rate: 1 Detector: UV 254 CHROMATOGRAM Retention time: k' 96.16

OTHER SUBSTANCES Also analyzed: acebutolol, alprenolol, antazoline, atenolol, betaxolol, bisoprolol, bopindolol, bupranolol, carteolol, celiprolol, chloropyramine, chlorpheniramine, cicloprolol, cimetidine, cinnarizine, cirazoline, clonidine, dilevalol, dimethindene, diphenhydramine, esmolol, famotidine, isothipendyl, ketotifen, metiamide, metoprolol, moxonidine, nadolol, naphazoline, nifenalol, nizatidine, oxprenolol, pheniramine, phentolamine, pindolol, pizotyline (pizotifen), practolol, prazosin, promethazine, propranolol, pyrilamine (mepyramine), ranitidine, roxatidine, sotalol, tiamenidine, timolol, tramazoline, tripelennamine, triprolidine, tymazoline, UK-14,304 REFERENCE
Kaliszan, R.; Nasal, A.; Turowski, M. Binding site for basic drugs on cti-acid glycoprotein as revealed by chemometric analysis of biochromatographic data. Biomed.Chromatogr., 1995, 9, 211215

SAMPLE Matrix: solutions HPLCVARIABLES Column: 125 X 5 5 |xm Spherisorb C8 Mobile phase: MeCN: water 25:45 containing 5 mM dibutylamine

Flow rate: 2
Detector: F ex 346 em 340 (filter) REFERENCE
Ferry, D.G.; Caplan, N.B.; Cubeddu, L.X. Interaction between antidepressants and alpha 1-adrenergic receptor antagonists on the binding to alpha 1-acid glycoprotein. J.Pharm.Sci., 1986, 75, 146-149