MICROBORE LIQUID-CHROMATOGRAPHY OF TERTIARY AMINE ANTICHOLINERGIC PHARMACEUTICALS WITH TRIS(2,2'-BI-PYRIDINE)RUTHENIUM(III) CHEMILUMINESCENCE DETECTION

被引:28
作者
HOLEMAN, JA [1 ]
DANIELSON, ND [1 ]
机构
[1] MIAMI UNIV,DEPT CHEM,OXFORD,OH 45056
基金
美国国家卫生研究院;
关键词
D O I
10.1093/chromsci/33.6.297
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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).
引用
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页码:297 / 302
页数:6
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