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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
Published:20 September 2019,
Published Online:04 April 2019,
Received:30 October 2018,
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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 25(18):145-149(2019)
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 25(18):145-149(2019) DOI: 10.13422/j.cnki.syfjx.20191414.
目的:
2
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:
2
采用UPLC BEH C
18
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:
2
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
(
r
=0.996 3),0.05~23.60 mg·L
-1
(
r
=0.995 5),0.09~18.60 mg·L
-1
(
r
=0.992 7),0.10~21.00 mg·L
-1
(
r
=0.998 8)和0.06~16.00 mg·L
-1
(
r
=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:
2
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。
Objective:
2
To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass for the determination of five biflavones.
Method:
2
Chromatographic separation was carried out on a ACQUITY UPLC BEH C
18
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:
2
Amentoflavone
bilobetin
ginkgetin
isoginkgetin
sciadopitysin showed a good linearity within the ranges of 0.02-13.20 mg·L
-1
(
r
=0.996 3)
0.05-23.60 mg·L
-1
(
r
=0.995 5)
0.09-18.60 mg·L
-1
(
r
=0.992 7)
0.10-21.00 mg·L
-1
(
r
=0.998 8)
0.06-16.00 mg·L
-1
(
r
=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:
2
The method was simple
and can be used for qualitative and quantitative analysis of biflavones.
超高效液相色谱串联三重四级杆质谱法银杏叶双黄酮树龄
UPLC-TQ-MSGinkgo biloba leavesbiflavonestree age
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