超高效液相色谱串联四级杆/静电场轨道阱高分辨质谱同时测定含银杏叶提取物保健食品中的萜类内酯和黄酮醇类成分  

Simultaneous determination of terpenoid lactones and flavonols in health food containing Ginkgo biloba L. extracts by ultra performance liquid chromatography-quadrupole/electrostatic field orbittrap high resolution mass spectrometry

作　　者：钮正睿[1] 郑天驰[1] 曹进[1] 李珉 丁宏[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]湖北省食品质量安全监督检验研究院,武汉430000

出　　处：《食品安全质量检测学报》2017年第7期2477-2485,共9页Journal of Food Safety and Quality

摘　　要：目的运用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry,UPLC-Q/OrbitrapHRMS),建立同时鉴别和定量测定含银杏叶提取物保健食品中的5种萜类内酯和3种黄酮醇类成分的分析方法。方法样品用80%甲醇水溶液提取,Acquity UPLC BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱分离,以甲醇和0.1%甲酸溶液作为流动相进行梯度洗脱,电喷雾负离子模式离子化,全扫描模式检测。结果槲皮素、山奈酚、异鼠李素、银杏内酯B、银杏内酯C、银杏内酯K和白果内酯在25~400μg/L范围内线性关系良好(r≥0.995),银杏内酯A在50~800μg/L范围内线性关系良好(r≥0.995)。8种成分的检出限在2~50 ng/g,定量限在8~150 ng/g之间。8种成分在含银杏叶提取物保健食品中均有较好的回收率和稳定性。结论该方法简便快速、灵敏准确,适合于含银杏叶提取物保健食品中的萜类内酯和黄酮醇类成分的鉴别和定量测定。Objective To establish a method for simultaneous determination of 5 terpenoid lactones and 3 flavonols in health food containing Ginkgo biloba extracts by ultra performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectrometry（UPLC-Q/OrbitrapHRMS）. Methods The samples were extracted with methanol：H_2O（80：20, V：V）, and separated on a Waters Acuity UPLC BEH C_（18） column（50 mm×2.1 mm, 1.7 μm） with methanol and 0.1% formic acid solution as mobile phase by gradient elution. The negative mode and full-scan method were used for detection. Results The linearities of quercetin, kaempferol, isorhamnetin, ginkgolide B, ginkgolide C, ginkgolide K and bilobalide were 25~400 μg/L, and the linearity of ginkgolide A was 50~800 μg/L. The correlation coefficients were all greater than 0.995. The limits of detection were 2~50 ng/g and the limits of quantification were 8~150 ng/g. The recoveries were 81.7%~106%, with the relative standard deviations in the range of 0.51% to 5.5%. Eight substances were stable in health food. Conclusion The established method can be used in screening and quantitative analysis of terpenoid lactones and flavonols in health foods.

关 键 词：超高效液相色谱-四极杆/静电场轨道阱高分辨质谱 银杏叶提取物 保健食品 萜类内酯 黄酮醇 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]