天然产物研究与开发 ›› 2023, Vol. 35 ›› Issue (5): 798-806.doi: 10.16333/j.1001-6880.2023.5.008

• 研究简报 • 上一篇    下一篇

超高效液相色谱串联质谱法同时测定乌药叶中6个黄酮类成分的含量

张煜炯,杨颖欣,刘京骅,孙崇鲁*   

  1. 浙江药科职业大学,宁波 315100
  • 出版日期:2023-05-26 发布日期:2023-05-26
  • 基金资助:
    浙江省药品监督管理局科技计划(2022009);宁波市“科技创新2025”重大专项(2019B10008)

Simultaneous determination of six flavonoids in Lindera aggregata leaf by UPLC-MS/MS

ZHANG Yu-jiong,YANG Ying-xin,LIU Jing-hua,SUN Chong-lu*   

  1. Zhejiang Pharmaceutical University,Ningbo 315100,China
  • Online:2023-05-26 Published:2023-05-26

摘要:

采用超高效液相色谱-串联质谱技术(UPLC-MS/MS)同时测定乌药叶中山柰酚-3-O-α-L-鼠李糖苷、槲皮素、槲皮素-3-O-β-D-木糖苷、槲皮素-3-O-α-L-阿拉伯呋喃糖苷、山柰酚-3-O-(2″-反式-对-香豆酰基)-α-L-鼠李糖苷、山柰酚-3-O-(2″,4″-二-反式-对-香豆酰基)-α-L-鼠李糖苷6个黄酮类化合物含量。采用Kinete XB-C18色谱柱(2.1 mm×50 mm,1.7 μm),流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱0~0.5 min,10%A;0.5~2 min,10%→30%A;2~6 min,30%→70%A;6~7min,70%→90%A;7~8 min,90%A;8~9 min,90%→10%A;9~10 min,10%A,流速为 0.2 ml/min,进样量1.0 μL,柱温30 ℃,采用电喷雾离子源(ESI),多反应监测(MRM),负离子扫描模式检测,结合熵权-TOPSIS法对10个产地的乌药叶进行分析评价。各化合物在一定浓度范围内线性良好,相关系数均大于0.999,加样回收率在98.15%~102.84%,RSD在0.60%~2.43%之间,经熵权-TOPSIS法分析评价,浙江天台产地乌药叶相对质量较好。该方法快速、灵敏度高、准确可靠,可为乌药叶中主要黄酮类化合物的定量分析及内在质量综合评价提供依据。

关键词: 乌药叶, UPLC-MS/MS, 化学成分, 含量测定, 熵权-TOPSIS法

Abstract:

Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used for the simultaneous determination of kaempferol-3-O-α-L-rhamnoside,quercetin,quercetin-3-O-β-D-xylopyranoside,quercetin-3-O-α-L-arabinofuranoside,kaempferol-3-O-(2″-E-p-coumaroyl)-α-L-rhamnoside and kaempferol-3-O-(2″,4″-di-E-p-coumaroyl)-α-L-rhamnoside of 6 flavonoids in Lindera aggregata leaf. Kinete XB-C18 column(2.1 mm×50 mm,1.7 μm) was used.The mobile phase was acetonitrile(A)-0.1% formic acid aqueous solution(B) in gradient elution mode(0-0.5 min,10% A;0.5-2 min,10%→30% A;2-6 min,30%→70% A;6-7 min,70%→90%A;7-8 min,90% A;8-9 min,90%→10%A;9-10min,10%A) with the flow rate of 0.2 mL/min.The injection volume was 1.0 μL and the column temperature was 30 ℃.Electrospray ionization source (ESI) and multiple reaction monitoring (MRM) were used combined with negative scanning switch.The linear relationship between the concentration and peak areas of the ten composition were all linear (r>0.999).The average recoveries were between 98.15%-102.84%,RSD were between 0.60%-2.43%.The entropy weight TOPSIS method was used to analyze and evaluate the relative quality of the L. aggregata leaf from Tiantai,Zhejiang.This method is rapid,sensitive,accurate and reliable,and can provide a basis for quantitative analysis and comprehensive evaluation of the internal quality of the main flavonoids in the L. aggregata leaf.

Key words: Lindera aggregata leaf, UPLC-MS/MS, chemical composition, content determination, entropy weight-TOPSIS method

中图分类号:  Q94