基于UPLC-TQ-MS考察不同树龄银杏叶双黄酮含量变化规律

郁丹红; 姜玮; 姚鑫; 薛平; 毛晨梅

doi:10.13422/j.cnki.syfjx.20191414

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基于UPLC-TQ-MS考察不同树龄银杏叶双黄酮含量变化规律

资源与质量评价 | 更新时间：2021-02-09

- 基于UPLC-TQ-MS考察不同树龄银杏叶双黄酮含量变化规律
- Determination of Biflavones in Ginkgo biloba Leaves of Different Ages by UPLC-TQ-MS
- 中国实验方剂学杂志 2019年25卷第18期页码：145-149
- 作者机构：
  
  1.苏州大学　附属儿童医院，江苏　苏州　 215000；
  2.泰州市食品药品检验所，江苏　泰州　 225300；
  3.苏州大学　附属第一医院，江苏　苏州　 215000；
  4.常州市食品药品监督检验中心，江苏　常州　 213000
- 作者简介：
  
  郁丹红，硕士，主管中药师，从事中药化学与分析研究，E-mail：yaobest@163.com
  毛晨梅，主任中药师，从事中药化学与分析研究，E-mail：chenmeimao@163.com
- 基金信息：
  
  江苏省食品药品监督管理局科研项目(20170218;20170226);苏州市科技发展计划项目(SYSD2017149)
- DOI：10.13422/j.cnki.syfjx.20191414
  中图分类号： R284.1; R289; R22; R2-031
- 收稿日期：2018-10-30，
  
  网络出版日期：2019-04-04，
  
  纸质出版日期：2019-09-20
- 稿件说明：
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郁丹红, 姜玮, 姚鑫, 等. 基于UPLC-TQ-MS考察不同树龄银杏叶双黄酮含量变化规律[J]. 中国实验方剂学杂志, 2019,25(18):145-149.

Dan-hong YU, Wei JIANG, Xin YAO, et al. Determination of Biflavones in Ginkgo biloba Leaves of Different Ages by UPLC-TQ-MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(18): 145-149.
郁丹红, 姜玮, 姚鑫, 等. 基于UPLC-TQ-MS考察不同树龄银杏叶双黄酮含量变化规律[J]. 中国实验方剂学杂志, 2019,25(18):145-149. DOI： 10.13422/j.cnki.syfjx.20191414.

Dan-hong YU, Wei JIANG, Xin YAO, et al. Determination of Biflavones in Ginkgo biloba Leaves of Different Ages by UPLC-TQ-MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(18): 145-149. DOI： 10.13422/j.cnki.syfjx.20191414.

摘要

目的：

建立超高效液相色谱串联三重四级杆质谱法同时测定银杏叶中5个双黄酮成分的含量。

方法：

采用UPLC BEH C

色谱柱(2.1 mm×100 mm，1.7 μm)，流动相0.10%甲酸溶液(A)-乙腈(B)，梯度洗脱(0～3 min，60%A；3～4 min，60%～50%A；4～6 min，50%A；6～8 min，50%～0A)，流速0.3 mL·min

－1

，柱温35 ℃，进样量1 μL。

结果：

穗花杉双黄酮、白果黄素、银杏素、异银杏素、金松双黄酮分别在0.02～13.20 mg·L

－1

(

＝0.996 3)，0.05～23.60 mg·L

－1

(

＝0.995 5)，0.09～18.60 mg·L

－1

(

＝0.992 7)，0.10～21.00 mg·L

－1

(

＝0.998 8)和0.06～16.00 mg·L

－1

(

＝0.996 7)线性关系良好。5个双黄酮加样回收率分别为101.50%，98.78%，97.59%，97.24%，101.09%，RSD分别为2.7%，2.7%，3.1%，2.8%，1.3%。银杏叶中双黄酮含量差异性较大，穗花杉双黄酮、白果黄素、银杏素、异银杏素、金松双黄酮的质量分数分别为121.30～434.74，268.39～847.14，251.80～1 297.10，195.87～691.10，477.48～3 003.90 μg·g

－1

，总双黄酮质量分数1 474.45～5 635.40 μg·g

－1

，但显示具有一定的规律性，即低树龄银杏叶含总双黄酮较高，随着树龄的增长，总双黄酮含量逐渐降低。

结论：

该方法专属性强，为银杏叶双黄酮类化合物的质量控制提供了一定的参考。

Abstract

Objective:

To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass for the determination of five biflavones.

Method:

Chromatographic separation was carried out on a ACQUITY UPLC BEH C

column (2.1 mm×100 mm

1.7 μm) with gradient elution of acetonitrile and 0.10%formic acid at a flow rate of 0.3 mL·min

-1

and the column temperature was set at 35 ℃.

Result:

Amentoflavone

bilobetin

ginkgetin

isoginkgetin

sciadopitysin showed a good linearity within the ranges of 0.02-13.20 mg·L

-1

(

=0.996 3)

0.05-23.60 mg·L

-1

(

=0.995 5)

0.09-18.60 mg·L

-1

(

=0.992 7)

0.10-21.00 mg·L

-1

(

=0.998 8)

0.06-16.00 mg·L

-1

(

=0.996 7)

with average recoveries of 101.50%

98.78%

97.59%

97.24%

101.09%

and RSDs of 2.7%

2.7%

3.1%

2.8%

1.3%. The contents of amentoflavone

bilobetin

ginkgetin

isoginkgetin

sciadopitysin ranged between 121.30-434.74

268.39-847.14

251.80-1 297.10

195.87-691.10

477.48-3 003.90 μg·g

-1

. The total biflavones ranged between 1 474.45-5 635.40 μg·g

-1

. It shows a certain regularity that the low-vinegar leaves contain higher total flavonoids

and the total flavonoid content gradually decreases with the increase of tree age.

Conclusion:

The method was simple

and can be used for qualitative and quantitative analysis of biflavones.

关键词

Keywords

references

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