Dicyclomine

Molecular formula: C19H35NO2 Molecular weight: 309.5 CAS Registry No.: 77-19-0 (dicyclomine), 67-92-5 (dicyclomine hydrochloride)

SAMPLE Matrix: blood Sample preparation: 2 mL Plasma + 100 JJIL 1 jxg/mL dicyclomine in water + 1 mL MeCN, vortex, allow to stand for 10 min, add 200 jxL 1 M pH 9.4 tris(hydroxymethyDmethylamine (TRIS), add 5 mL hexane, shake horizontally for 10 min, centrifuge at 2000 g for 5 min. Remove the aqueous layer and add it to 3 mL hexane, shake horizontally for 10 min, centrifuge at 2000 g for 5 min. Combine the hexane layers and add them to 1 mL 100 mM HCl, shake for 10 min, centrifuge. Remove the aqueous layer and evaporate it to dryness under vacuum, reconstitute in 250 |JLL mobile phase, inject a 100 jjiL aliquot. HPLCVARIABLES Column: 100 mm long 5 |xm Techsil CN Mobile phase: MeOH: 20 mM pH 6.2 orthophosphoric acid buffer 40:60 Column temperature: 30 Flow rate: 0.6 Injection volume: 100 Detector: E, ESA Coulochem 5100-A, guard cell 1.0 V, dual porous graphite electrode 0.85 and 0.95 V CHROMATOGRAM Retention time: 23 Internal standard: dicyclomine OTHER SUBSTANCES Extracted: oxybutynin KEYWORDS plasma; dicyclomine is IS REFERENCE
Hughes, K.M.; Lang, J.C.T.; Lazare, R.; Gordon, D.; Stanton, S.L.; Malone-Lee, J.; Geraint, M. Measurement of oxybutynin and its N-desethyl metabolite in plasma, and its application to pharmacokinetic studies in young, elderly and frail elderly volunteers. Xenobiotica, 1992, 22, 859-869

SAMPLE
Matrix: solutions

HPLCVARIABLES Column: 150 X 2 Deltabond C8 (Keystone) Mobile phase: MeCN: 2-butanone: 50 mM pH 7.0 phosphate buffer 27:13:60 Flow rate: 0.15 Injection volume: 1 Detector: Chemiluminescence following post-column reaction. A 1 mM solution of Ru(2,2'bipyridine)32+ in 50 mM sodium sulfate (continuously sparged with helium) was oxidized to Ru(2,2'-bipyridine)33+ using a Princeton Applied Research Model 174A polarographic

analyzer with a platinum gauze working electrode, a platinum wire auxiliary electrode, and a silver wire reference electrode. The Ru solution was pumped at 0.3 mL/min and mixed with the column effluent in the flow cell of the detector, a fluorescence detector with the light source removed.
CHROMATOGRAM

Retention time: 14 Limit of detection: 0.1-1 /xg/mL OTHER SUBSTANCES Simultaneous: cyclobenzaprine KEYWORDS post-column reaction REFERENCE
Holeman, J.A.; Danielson, N.D. Microbore liquid chromatography of tertiary amine anticholinergic pharmaceuticals with tris(2,2'-bipyridine)ruthenium(III) chemiluminescence detection. J.Chromatogr. ScL, 1995, 33, 297-302

SAMPLE Matrix: solutions Sample preparation: Prepare a 10 |xg/mL solution in MeOH, inject a 20 yJu aliquot. HPLCVARIABLES Column: 125 X 4.9 Spherisorb S5W silica Mobile phase: MeOH containing 10 mM ammonium perchlorate and 1 mL/L 100 mM NaOH in MeOH, pH 6.7 Flow rate: 2 Injection volume: 20 Detector: E, LeCarbone, V25 glassy carbon electrode, + 1.2 V
CHROMATOGRAM

Retention time: 1.8

OTHER SUBSTANCES Also analyzed: acebutolol, acepromazine, acetophenazine, N-acetylprocainamide, albuterol, alprenolol, amethocaine, amiodarone, amitriptyline, antazoline, atenolol, azacyclonal, bamethane, benactyzine, benperidol, benzethidine, benzocaine, benzoctamine, benzphetamine, benzquinamide, bromhexine, bromodiphenhydramine, bromperidol, brompheniramine, brompromazine, buclizine, bufotenine, bupivacaine, buprenorphine, butacaine, butethamate, chloreyclizine, chlorpheniramine, chlorphenoxamine, chlorprenaline, chlorpromazine, chlorprothixene, cimetidine, cinchonidine, cinnarizine, clemastine, clomipramine, clonidine, cocaine, cyclazocine, cyclizine, cyclopentamine, cyproheptadine, deserpidine, desipramine, dextromoramide, dextropropoxyphene, diethylcarbamazine, diethylpropion, diethylthiambutene, dihydroergotamine, dimethindene, dimethothiazine, diphenhydramine, diphenoxylate, dipipanone, diprenorphine, dipyridamole, disopyramide, dothiepin, doxapram, doxepin, doxylamine, droperidol, ephedrine, ergocornine, ergocristine, ergocristinine, ergocryptine, ergometrine, ergosine, ergosinine, ergotamine, ethopropazine, etorphine, etoxeridine, fenethazine, fenfluramine, fenoterol, fentanyl, flavoxate, fluopromazine, flupenthixol, fluphenazine, flurazepam, haloperidol, hydroxyzine, hyoscine, ibogaine, imipramine, indapamine, iprindole, isothipendyl, isoxsuprine, ketanserin, laudanosine, lidocaine, lofepramine, loxapine, maprotiline, mecamylamine, meclophenoxate, meclozine, medazepam, mephentermine, mepivacaine, meptazinol, mepyramine, mesoridazine, metaraminol, methadone, methamphetamine, methapyrilene, methdilazene, methotrimeprazine, methoxamine, methoxyphenamine, methoxypromazine, methylephedrine, methylergonovine, methysergide, metoclopramide, metopimazine,

metoprolol, mianserin, morazone, nadolol, nalorphine, naloxone, naphazoline, nicotine, nifedipine, nomifensine, nortriptyline, noscapine, orphenadrine, oxeladin, oxprenolol, oxymetazolin, papaverine, pargyline, pecazine, penbutolol, pentazocine, penthienate, pericyazine, perphenazine, phenadoxone, phenampromide, phenazocine, phenbutrazate, phendimetrazine, phenelzine, phenglutarimide, phenindamine, pheniramine, phenmetrazine, phenomorphan, phenoperidine, phenothiazine, phenoxybenzamine, phentolamine, phenylephrine, phenyltoloxamine, physostigmine, piminodine, pimozide, pindolol, pipamazine, pipazethate, piperacetazine, piperidolate, pipradol, pirenzepine, piritramide, pizotifen, practolol, pramoxine, prazosin, prenylamine, prilocaine, primaquine, proadifen, procainamide, procaine, prochlorperazine, procyclidine, proheptazine, prolintane, promazine, promethazine, pronethalol, properidine, propiomazine, propranolol, prothipendyl, protriptyline, proxymetacaine, pseudoephedrine, pyrimethamine, quinidine, quinine, ranitidine, rescinnamine, sotalol, tacrine, terazosin, terbutaline, terfenadine, thenyldiamine, theophylline, thiethylperazine, thiopropazate, thioproperazine, thioridazine, thiothixene, thonzylamine, timolol, tocainide, tolpropamine, tolycaine, tranylcypromine, trazodone, trifluoperazine, trifluperidol, trimeperidine, trimeprazine, trimethobenzamide, trimethoprim, trimipramine, tripelennamine, triprolidine, tryptamine, verapamil, xylometazoline REFERENCE
Jane, L; McKinnon, A.; Flanagan, R. J. High-performance liquid chromatographic analysis of basic drugs on silica columns using non-aqueous ionic eluents. II. Application of UV, fluorescence and electrochemical oxidation detection. J.Chromatogr., 1985, 323, 191-225