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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。
OBJECTIVE To establish a method for the simultaneous determination of alkaloids in lotus leaf by SPE-RRLC-Q-TOF combined with rapid separation liquid-liquid phase-quadrupole time-of-flight mass spectrometry. Methods The samples were extracted with 1% hydrochloric acid by ultrasonic extraction and cleaned up by solid phase extraction (SPE) cartridge. Then, the sample was eluted with ammonia-methanol. The eluate was concentrated and fixed with methanol. Welch Materials C18 column was used for gradient elution with acetonitrile-water as mobile phase. The analytes were separated by fast liquid phase-time-of-flight mass spectrometry (RRLC-Q-TOF) in positive ion mode. Results Nine alkaloids were isolated and tested. Conclusion Rapid separation of liquid phase - quadrupole time of flight mass spectrometry combined with cation exchange SPE column pretreatment technology can quickly and accurately identify alkaloids in lotus leaf.