title: Microbore liquid chromatography of tertiary amine anticholinergic pharmaceuticals with tris(2,2'-bipyridine)ruthenium(III) chemiluminescence detection.
abstract: The post-column chemiluminescent reaction of six anticholinergic alkaloid compounds with tris(2,2'-bipyridine)ruthenium(III) (Ru(bpy)3(3+)) is applied to microbore high-performance liquid chromatography (HPLC). At flow rates less than 200 microL/min, the capillary mixing cell in which Ru(bpy)3(3+) and the analyte are mixed directly allows for good light detection. In contrast, a diminished signal occurs at these low flow rates with conventional post-column mixing in a tee. Optimal chemiluminescent pH conditions for atropine, scopolamine, dicyclomine, cyclopentolate, cyclobenzaprine, and procyclidine are determined at moderately basic conditions (pH 7 to 9). 2-Butanone is found to be compatible with the chemiluminescent reaction, whereas tetrahydrofuran and propionitrile cause an increase in background noise and a chemiluminescent signal loss. As 2-butanone is more nonpolar than acetonitrile, it assists in the elution of these hydrophobic anticholinergic compounds. Five anticholinergic compounds are resolved successfully with a PRP-1 polymeric column and a slightly basic mobile phase, but a C8 silica column is better suited for the more hydrophobic compounds (cyclobenzaprine, procyclidine, and dicyclomine).
authors.affiliation: Department of Chemistry, Miami University, Oxford, Ohio 45056, USA.
authors.forename: J A
authors.initials: JA
authors.lastname: Holeman
authors.forename: N D
authors.initials: ND
authors.lastname: Danielson
mesh_terms: D015082:2,2'-Dipyridyl / Q000031:analogs & derivatives*; D000588:Amines / Q000302:isolation & purification*; D000639:Amitriptyline / Q000031:analogs & derivatives / Q000302:isolation & purification; D001285:Atropine / Q000302:isolation & purification; D002074:Butanones; D018680:Cholinergic Antagonists / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003519:Cyclopentolate / Q000302:isolation & purification; D004025:Dicyclomine / Q000302:isolation & purification; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents; D008163:Luminescent Measurements; D009942:Organometallic Compounds; D011352:Procyclidine / Q000302:isolation & purification; D012601:Scopolamine / Q000302:isolation & purification
chemical_list: D000588:Amines; D002074:Butanones; D018680:Cholinergic Antagonists; D007202:Indicators and Reagents; D009942:Organometallic Compounds; D000639:Amitriptyline; C058901:tris(2,2'-bipyridine)ruthenium III; D004025:Dicyclomine; D015082:2,2'-Dipyridyl; C004704:cyclobenzaprine; C005222:methylethyl ketone; D001285:Atropine; D011352:Procyclidine; D012601:Scopolamine; D003519:Cyclopentolate