YAO Xin, XUE Ping, YU Dan-hong, et al. Determination of Ginkgolic Acids in Ginkgo Leaves Extract from Different Manufacturers by UPLC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(18): 174-179.
DOI:
YAO Xin, XUE Ping, YU Dan-hong, et al. Determination of Ginkgolic Acids in Ginkgo Leaves Extract from Different Manufacturers by UPLC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2017, 23(18): 174-179. DOI: 10.13422/j.cnki.syfjx.201718000.
Determination of Ginkgolic Acids in Ginkgo Leaves Extract from Different Manufacturers by UPLC-MS/MS
Objective: To establish UPLC-MS/MS for simultaneous determination of five ginkgolic acids in ginkgo leaves extract.Method: UPLC BEH C18 column (2.1 mm×100 mm
1.7 μm) was used with methanol-0.1% formic acid solution as the mobile phase for gradient elution. The flow rate was 0.4 mL · min-1 with 30℃ column temperature; the mass spectrometer monitors were used to detect related ions by multiple reaction ion monitoring (MRM) mode.Result: The hydroginkgoic acid
ginkgoneolic acid
oleanolic acid
dioctylmethane allyl ginkgolic acid
and dioctylmethane diallyl ginkgolic acid were well separated within 5.0 min
showing good linear relationship (r>0.992 3) at the ranges of 0.20-200.00 ng · L-1. RSD value of the average recoveries was below 5.0% which ranged from 98.86% to 103.30%. We found that the content of the five ginkgolic acids in ginkgo leaves extract from different manufacturers was very different (7.58-23.08 μg ·g-1). The highest content of determined ginkgolic acids in one manufacturer was more than 20 ppm. Only 8 companies met the requirements of the state pharmacopoeia commission of P.R. China (below 10 ppm). ginkgo leaves extract produced by different manufacturers in the market generally had high levels of ginkgolic acid. The contents of ginkgoneolic acid
oleanolic acid
and dioctylmethane allyl ginkgolic acid were higher
while the contents of hydroginkgoic acid and dioctylmethane diallyl ginkgolic acid were lower. According to the results of ginkgo leaves extract from eight qualified manufacturers
we suggested that the contents should be controlled at 2.94-3.59
0.97-1.18
2.35-2.88
2.94-3.59
0.59-0.73 μg ·g-1 respectively for hydroginkgoic acid
ginkgoneolic acid
oleanolic acid
dioctylmethane allyl ginkgolic acid
and dioctylmethane diallyl ginkgolic acid.Conclusion: This method can be used for the quick analysis of ginkgolic acids.