基于UPLC-Q-TOF-MS的砂糖橘皮化学成分分析  

Qualitative Analysis of Chemical Constituents in Citrus reticulata 'Shiyue Ju' by UPLC-Q-TOF-MS

作　　者：罗美霞[1] 吴波[1] 胡坪君 韦敏燕[1] 杨秀娟 刘鄂湖[2] 郑国栋[1] 

机构地区：[1]广州医科大学,广州511436 [2]中国药科大学,南京211198

出　　处：《中国实验方剂学杂志》2017年第21期45-51,共7页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家自然科学基金青年基金项目(31401613);2014年广东省高校优秀青年培养计划项目(粤教师函[2014]145号);广州市属高校科研计划项目(2012C210)

摘　　要：目的:通过超高效液相色谱串联-四级杆-飞行时间质谱(UPLC-Q-TOF-MS)联用技术对砂糖橘果皮化学成分进行快速分析和鉴定。方法:采用Aglient Zorbax Extend C_(18)色谱柱(4.6 mm×50 mm,1.8μm),以0.1%甲酸水(A)-乙腈(B)为流动相,梯度洗脱进行色谱分离,流速0.6 m L·min^(-1),柱温35℃,进样体积0.5μL。飞行时间质谱,采用电喷雾(ESI)离子源,在正离子模式下采集数据,质量扫描范围设置为m/z 100~1 000,运行时间24 min,使用质谱分析软件Peak view中的目标化合物筛查法,结合保留时间、精确相对分子质量和二级质谱裂解碎片鉴定和推测成分。结果:在所设定的LC-MS条件下,结合对照品及文献报道的质谱数据对砂糖橘果皮的甲醇提取液分析,共分离鉴定了31个成分,包括5个黄酮碳苷,6个黄酮氧苷,17个多甲氧基黄酮,1个生物碱和2个多酚类化合物。结论:研究中建立的检测方法简便、准确,为快速鉴定分析化学成分提供一种有效的分析方法,并比较全面地阐明了砂糖橘果皮化学组成,这为砂糖橘果皮成为供开发利用的柑橘资源提供科学依据。Objective ： To analyze and evaluate the chemical constituents of Citrus reticulata ＇ Shiyue Ju＇ rapidly by using ultra-high performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry （UPLC-Q-TOF-MS） technique. Method： The LC separation was performed on a UPLC Aglient Zorbax Extend C18column （4.6 mm × 50 mm, 1.8 μm） , with 0. 1% formic acid solution （A） -acetonitrile solution （ B ） as the mobile phase for gradient elution. The flow rate was 0.6 mL-min- 1 ; column temperature was set at 35 ℃ ; and injection volume was 0.5 μL. Electrospray ion （ESI） source was applied for the TOF-MS analysis under the positive ion mode; the mass scanning range was between m/z 100-1 000; and the running time was 24 min. By using target compound screening method in the mass spectrometry analysis software, the structures of monitoredchemical compositions were identified and speculated by retention time, exact relative molecular weight and the secondary mass spectra fragment of MS. Result： Under certain chromatographic conditions, thirty-one chemical compounds were separated and identified completely from the methanol extraction of C. reticulata ＇Shiyue Ju＇ based on reference substances and related references, including five flavone C-glycosides, six flavone O-glycosides, seventeen polymethoxylated flavonoids （PMFs）, alkaloid and two polyphenols compounds. Conclusion： The established detection method was convenient and accurate, providing an analytical approach for rapidly identifying and analyzing the chemical compounds. The study supplied the scientific basis to become available for the development and utilization of citrus resources.

关 键 词：砂糖橘 超高效液相色谱串联-四级杆飞行时间质谱 化学成分 

分 类 号：R284.1[医药卫生—中药学]