固相萃取快速分离液相四级杆串联飞行时间质谱联用分析荷叶中概要.docVIP

中草药 Chinese Traditional and Herbal Drugs 第 42卷 第 6期 2011年 6月 ? 1066? 固相萃取 -快速分离液相 -四级杆串联飞行时间质谱联用分析荷叶中的生物碱 郑振佳 1, 2,王 晓 2*,王明林 1,王珊珊 2,赵先恩 2 1. 山东农业大学食品科学与工程学院,山东 泰安 271018 2. 山东省科学院 中药过程控制研究中心,山东省分析测试中心,山东 济南 250014 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。 关键词:固相萃取;快速分离液相 -四级杆串联飞行时间质谱;荷叶;生物碱;阳离子交换 中图分类号:R284.1 文献标志码:A 文章编号:0253 -2670(201106 - 1066 - 03 Analysis of alkaloids in Nelumbo nucifera leaves by solid phase extraction-rapid resolution liquid chromatography-quadrupole-time of flight mass spectrometry ZHENG Zhen-jia1, 2, WANG Xiao2, WANG Ming-lin1, WANG Shan-shan2, ZHAO Xian-en2 1. College of Food Science and Engineering, Shandong Agricultural University, Taian 271018, China 2. Process Control Research Center of Traditional Chinese Medicine, Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan 250014, China 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. Key words: solid phase extraction (SPE; rapid resolution liquid chromatography-quadrupole-time of flight (RRLC-Q-TOF mass spectrometry; Nel