Determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by mix-mode SPE-UHPLC/MS/MS
10.16438/j.0513-4870.2018-0248
- VernacularTitle:混合型固相萃取-UHPLC/MS/MS法测定银杏酮酯滴丸中银杏酸含量
- Author:
Jian SUN
1
;
Xue-yi ZHANG
2
;
Li-min LI
1
;
Qing HU
1
;
Yan-rong ZHU
1
;
Xiu-hong MAO
1
;
Shen JI
1
Author Information
1. Shanghai Institute for Food and Drug Control, Shanghai 201203, China
2. Shanghai Shangyao Xingling Technology Pharmaceutical Co., Ltd., Shanghai 201703, China
- Publication Type:ORIGINAL ARTICLES
- Keywords:
ultra high performance liquid chromatography-tandem mass spectrometry;
mix-mode solidphase extraction;
ginkgolic acid;
Yinxing Tongzhi Dropping Pills
- From:
Acta Pharmaceutica Sinica
2018;53(9):1532-1535
- CountryChina
- Language:Chinese
-
Abstract:
An analytical method was developed for determination of ginkgolic acids in Yinxing Tongzhi Dropping Pills by ultra high performance liquid chromatography-triple quadrupole mass spectrometry. The samples were purified by mix-mode anion exchange and reversed-phase SPE. A chromatographic column, Waters Cortecs T3 (50 mm×2.1 mm, 2.7 μm), was used with acetonitrile-methanol-1% acetic acid (44:44:12) as the mobile phase. The ginkgolic acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring (MRM) mode. Ginkgolic acid C13:0, C15:1 and C17:1 possessed good linear correlation in the mass concentration range from 0.2 to 200 μg·L-1, 2 to 200 μg·L-1, 4 to 200 μg·L-1, respectively, with the correlation coefficients more than 0.999. The mean recoveries at spiked levels of 50, 250 and 600 μg·kg-1 were in the range of 70.8%-95.1%, and the RSDs were 0.7%-8.6%. The limits of quantification were 1, 10, 20 μg·kg-1, respectively. The method could be applied to the analysis of ginkgolic acids in complex matrix samples.
