Wang Shufang, Qu Haibin, Cheng Yiyu
Pharmaceutical Informatics Institute, Zhejiang University, Hangzhou, P. R. China.
Electrophoresis. 2007 May;28(9):1399-406. doi: 10.1002/elps.200600428.
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.
建立了一种快速、可重复且高灵敏度的非水毛细管电泳-电喷雾电离质谱（NACE-ESI-MS）方法，用于分析苦参和越南槐根中的槐定碱、苦参碱、槐果碱和氧化苦参碱。场放大进样堆积结合电迁移进样（FASS-EMI）首次用于NACE中生物碱的在线富集。系统优化了NACE分离、FASS-EMI堆积和MS检测的条件。最佳的NACE缓冲液是一种含有50 mM醋酸铵、0.5%乙酸和30%乙腈（溶于甲醇）的电解质。FASS-EMI技术使灵敏度提高了约100倍，MS检测进一步将其提高了1000倍以上。各峰相对迁移时间和相对峰面积的日内RSD（n = 6）分别小于0.3%和2.4%，日间RSD分别小于5.1%和6.0%。分析物的检测限（S/N = 3）为0.0210 - 0.0446 ng/mL。基于这种NACE-ESI-MS方法，在有效去除离子后，可能开发一种生物分析方法用于分析生物样品基质（血浆、尿液等）中的生物碱。
