[关键词]
[摘要]
目的 建立固相萃取-快速分离液相-四级杆串联飞行时间质谱(SPE-RRLC-Q-TOF)联用技术分析荷叶中的生物碱类化合物的方法。方法 样品采用1%盐酸超声提取,经固相萃取(SPE)小柱净化,再用氨水-甲醇进行洗脱,洗脱液浓缩后用甲醇定容。选用Welch Materials C18柱,以乙腈-水为流动相进行梯度洗脱,在正离子模式下,经快速分离液相-飞行时间质谱(RRLC-Q-TOF)分析。结果 分离并检测了9种生物碱。结论 快速分离液相-四级杆串联飞行时间质谱结合阳离子交换固相萃取柱前处理技术,可以快速准确鉴定荷叶中的生物碱成分。
[Key word]
[Abstract]
Objective A novel method for the analysis of alkaloids in Nelumbo nucifera leaves was established by SPE-RRLC-Q-TOF mass spectrometry. Methods The crude sample was extracted by 1% HCl with ultrasound-assisted extraction, then purified by SPE column, and eluted with ammonia-methanol (5:95). After concentration, the residue was dissolved by methanol solution. The real sample was analyzed by RRLC-Q-TOF. A Welch Materials C18 column was applied in the RRLC separation using acetonitrile and water as mobile phase. The elutes were detected by Q-TOF to obtain the MS spectra with extract molecular weights under positive ion mode. Results Nine alkaloids were identified. Conclusion This method can be used to rapidly determine the alkaloids of N. nucifera leaves.
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[基金项目]
国家自然科学基金资助项目(20872083);山东省科技攻关项目(2009GG2001021-16);山东省科学院博士基金项目(科基合字2010第22号);济南市高校院所自主创新计划(201004010)