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纸质出版日期:2017
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姚鑫, 薛平, 郁丹红, 等. UPLC-MS/MS测定银杏叶提取物中5种微量银杏酸[J]. 中国实验方剂学杂志, 2017,23(18):174-179.
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.
姚鑫, 薛平, 郁丹红, 等. UPLC-MS/MS测定银杏叶提取物中5种微量银杏酸[J]. 中国实验方剂学杂志, 2017,23(18):174-179. DOI: 10.13422/j.cnki.syfjx.201718000.
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.
目的:建立UPLC-MS/MS同时测定银杏叶提取物中5种微量银杏酸的方法。方法:以UPLC BEH C18(2.1 mm×100 mm,1.7 μm)为色谱柱,甲醇-0.1%甲酸水溶液为流动相,流速0.4 mL · min-1,柱温30℃;质谱仪以多反应离子监测(MRM)方式进行相关离子检测。结果:测定的氢化白果酸、白果新酸、白果酸、十七烷一烯银杏酸以及十七烷二烯银杏酸在5.0 min内分离良好,在测定的质量浓度范围内(0.20~200.00 μg · L-1)线性关系良好(r>0.992 3);加样回收率(n=6) RSD均<5%(98.86%~103.30%)。不同厂家银杏叶提取物中的银杏酸含量差异较大(7.58~23.08 μg ·g-1),最高含量高达百万分之二十以上,仅有8家提取物低于百万分之十,市面不同厂家生产的银杏叶提取物普遍银杏酸含量偏高。在所测定的各批次样品中白果酸、十七烷一烯银杏酸以及中白果新酸平均含量较高,十七烷二烯银杏酸和氢化白果酸平均含量较低。根据8家合格银杏叶提取物厂家的测定结果,建议所测定的5种银杏酸即:氢化白果酸、白果新酸、白果酸、十七烷一烯银杏酸以及十七烷二烯银杏酸的质控范围分别控制在2.94~3.59,0.97~1.18,2.35~2.88,2.94~3.59,0.59~0.73 μg ·g-1。结论:该方法可用于银杏酸类成分的快速定量分析。
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.
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