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NACE‐ESI‐MS combined with on‐line concentration for high‐sensitivity analysis of quinolizidine alkaloids
Author(s) -
Wang Shufang,
Qu Haibin,
Cheng Yiyu
Publication year - 2007
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.200600428
Subject(s) - chromatography , chemistry , quinolizidine , oxymatrine , analyte , acetic acid , sophora flavescens , isotachophoresis , matrine , bioanalysis , ammonium acetate , electrolyte , alkaloid , high performance liquid chromatography , stereochemistry , organic chemistry , electrode
Abstract A rapid, reproducible and high‐sensitivity NACE‐ESI‐MS method was developed for the analysis of sophoridine, matrine, sophocarpine and oxymatrine in the roots of Sophora flavescens Ait. and S. tonkinensis Gagnep. Field‐amplified sample stacking with electromigration‐injection (FASS‐EMI) was first used in NACE for the on‐line concentration of the alkaloids. The conditions of NACE separation, FASS‐EMI stacking and MS detection were systematically optimized. The optimum NACE buffer was an electrolyte containing 50 mM ammonium acetate, 0.5% acetic acid and 30% ACN in methanol. The sensitivity was improved by about 100‐fold by the FASS‐EMI technique, which was further improved by more than 1000‐fold with MS detection. The RSDs ( n = 6) of the relative migration time and relative peak area of each peak were less than 0.3 and 2.4% for intra‐day and less than 5.1 and 6.0% for inter‐day, respectively. The LODs (S/N = 3) of analytes were determined to be 0.0210–0.0446 ng/mL. A bioanalytical method based on this NACE‐ESI‐MS method may be developed for the analysis of the alkaloids in biological sample matrices (plasma, urine, etc. ) after effective ion removal.