Islam Nurul M, Yoo Hye Hyun, Lee Min Woo, Dong Mi-Sook, Park Young In, Jeong Ha Sook, Kim Dong-Hyun
Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology, Seoul 130-650, Korea.
Phytochem Anal. 2008 Jan-Feb;19(1):71-7. doi: 10.1002/pca.1018.
A rapid and accurate reversed-phase liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been developed and validated for the quantitative determination of five flavonoid glycosides, icariin, epimedin A, epimedin B, epimedin C and hyperin in Herba Epimedii. Chromatographic separations were performed using a C(18) narrow-bore HPLC column; a mixture of an aqueous solution of ammonium formate (pH 4.0) and acetonitrile was used as the mobile phase, with compounds detected in the positive ion mode with multiple-reaction monitoring using a triple-quadrupole mass spectrometer equipped with an electrospray ionisation interface. This method for the determination of the reported flavonoid glycosides was accurate and reproducible, with a lower limit of quantication of 0.5 microg/mL. The standard calibration curves for the above-mentioned compounds were linear (r(2) > 0.998) over the concentration range 0.5-10.0 microg/mL. The relative standard deviations for intra- and inter-day precision over the concentration range for the flavonoid glycosides were lower than 7.8% with accuracy between 90.1 and 111.0%. The established method was successfully applied to the quality assessment of samples of Herba Epimedii collected from Korea and China.
已开发并验证了一种快速准确的反相液相色谱 - 串联质谱法（HPLC - MS/MS），用于定量测定淫羊藿中五种黄酮苷，即淫羊藿苷、朝藿定A、朝藿定B、朝藿定C和金丝桃苷。色谱分离采用C(18)窄径HPLC柱；以甲酸铵水溶液（pH 4.0）和乙腈的混合物为流动相，使用配备电喷雾电离接口的三重四极杆质谱仪在正离子模式下通过多反应监测检测化合物。该测定所报道黄酮苷的方法准确且可重现，定量下限为0.5 μg/mL。上述化合物的标准校准曲线在0.5 - 10.0 μg/mL浓度范围内呈线性（r(2) > 0.998）。黄酮苷浓度范围内日内和日间精密度的相对标准偏差低于7.8%，准确度在90.1%至111.0%之间。所建立的方法成功应用于从韩国和中国采集的淫羊藿样品的质量评估。
