基于UPLC-TQ-MS考察不同树龄果用银杏叶萜内酯含量变化规律  

Determination of terpene lactones in Ginkgo biloba leaves in different ages by UPLC-TQ-MS

作　　者：姚鑫[1] 周桂生[1] 唐于平[1] 钱叶飞[1] 尚尔鑫[1] 宿树兰[1] 钱大玮[1] 段金廒[1] 

机构地区：[1]南京中医药大学江苏省方剂高技术研究重点实验室,江苏南京210046

出　　处：《中国中药杂志》2013年第3期376-380,共5页China Journal of Chinese Materia Medica

基　　金：国家科技支撑计划项目(2011BAI04B03);国家教育部"新世纪优秀人才支持计划"项目(NCET-09-0163);江苏高校优势学科建设工程项目(ysxk-2010)

摘　　要：目的:建立超高效液相色谱串联三重四级杆质谱法(UPLC-TQ-MS)同时测定银杏叶中4个萜内酯成分的含量。方法:采用ACQUITYTMUPLC BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,以水(A)-甲醇(B)为流动相,等度洗脱(70%A),流速0.4 mL.min-1,柱温30℃;Waters XevoTMTQ质谱仪以多反应离子监测(MRM)方式进行负离子检测。结果:各成分在5.0 min内分离良好,在相应的浓度范围内与峰面积呈良好的线性关系,相关系数均>0.990 3;加样回收率(n=6)为98.83%～103.9%,RSD均小于3%。不同树龄果用银杏叶中萜内酯的含量差异较大,低树龄银杏叶含总内酯较高,随着树龄的增长,内酯含量逐渐降低。结论:该方法简便、快速、重复性好、专属性强,适用于银杏叶中萜内酯类成分的快速定量分析。Objective： To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass （ UP- LC-TQ-MS） for determination of four terpene lactones. Method： Chromatographic separation was carried out on a ACQUITY UPLC BEH Cls column （2.1 mm× 100 ram, 1.7 μm） with isocratic elution of 70% methanol at a flow rate of 0.4 mL min-1, the column temperature was set at 30 ℃ ; Waters XevoTM TQ worked in multiple reaction monitoring mode. Result： All calibration curves were lin- ear （ r 〉 0. 990 3） over the tested ranges. The average recoveries ranged from 98.83% to 103.9% with RSD value below 3.0%. The contents of total terpene lactones in Ginkgo biloba leaves were significantly different in different ages. The contents in the leaves of young ginkgo tree were higher than that in old tree. Conclusion： The method was simple and fast with high precision, sensitivity and repeatability, which can be used for qualitative and quantitative analysis of terpene lactones in G. biloba leaves.

关 键 词：UPLC—TQ—MS 果用银杏叶 萜内酯 树龄 

分 类 号：R284[医药卫生—中药学]