建立了超高效液相色谱-串联三重四极杆质谱测定银杏叶提取物及其制剂中银杏酸的方法.采用 Agilent Poroshell 120 EC-C18色谱柱(50 mm×3. 0 mm,2. 7 μm),以甲醇-1%冰醋酸溶液(90:10,v/v)为流动相,在电喷雾离子化负离子模式下,以多反应监测方式( MRM)检测.银杏酸 C13:0、C15:1、C17:1 在 2~200 μg/L 范围内呈良好的线性关系,相关系数均大于0. 999;在5、20和100 μg/L加标水平下的平均加样回收率为86. 3%~114. 3%,相对标准偏差( RSD)为0. 5%~13. 6%;检出限为0. 003~0. 08 μg/g,定量限为 0. 01~0. 19 μg/g.本方法已应用于实际样品的测定.
An analytical method was developed for the determination of ginkgolic acids in ginkgo biloba extract and its preparations by ultra high performance liquid chromatography-triple quadrupole mass spectrometry. A chromatographic column,Agilent Poroshell 120 EC-C18 (50 mm×3. 0 mm,2. 7 μm),was used with methanol-1% acetic acid(90 :10,v/v)as the mobile phase. The ginkgo acids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring( MRM)mode. Ginkgo acids C13:0,C15:1 and C17:1 possessed good linear correlations in the mass concentration range from 2 to 200 μg/L, with the correlation coefficients more than 0. 999. The mean recoveries at the spiked levels of 5, 20 and 100 μg/L were in the range of 86. 3%-114. 3%,and the RSDs were 0. 5%-13. 6%. The limits of detection and quantification were 0. 003-0. 08 μg/g and 0. 01-0. 19 μg/g,respectively. The method was successfully applied to the analysis of actual samples.
参考文献
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%