摘要
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,2.7μm）,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2~200μg/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100μg/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0.003~0.08μg/g,定量限为0.01~0.19μg/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 chromatographytriple 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.
出处
《色谱》
CAS
CSCD
北大核心
2016年第2期184-188,共5页
Chinese Journal of Chromatography
基金
2015年上海市食品药品监督管理局技术类专项课题~~
关键词
超高效液相色谱-三重四极杆质谱
银杏酸
银杏叶提取物
银杏叶片
银杏叶胶囊
ultra high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/ MS）
ginkgolic acid
ginkgo biloba extract
ginkgo leaf tablet
ginkgo leaf capsule
