Zhang Shuangqing, He Mengjie, Huang Zhenwu
National Institute for Nutrition and Health, Chinese Center for Disease Control and Prevention, Beijing 100050, China.
Wei Sheng Yan Jiu. 2016 Sep;45(5):807-810.
To establish an ultra-performance liquid chromatographytandem mass spectrometry( UPLC-MS / MS) method for the quantification of icariin( ICA), and investigate pharmacokinetics of ICA in rats following multiple oral administration.
ICA and an internal standard coumestrol( CMT) were extracted from rat plasma using ethyl acetate and separated on a BEH C18( 50 mm × 2. 1mm, 1. 7 μm) column using a gradient mobile phase of acetonitrile containing 0. 1%( V / V)formic acid and water containing 2 mmol / L ammonium formate at a flow rate of 0. 3m L / min. In negative electrospray ionization mode, multiple reaction monitoring of the precursor-product ion transitions of m / z 675. 6→351. 1 for ICA, 267. 0 →211. 1 for CMT was used for the quantification. Plasma was collected after rats were orally administered with ICA at multiple doses of 50 mg / kg.
The linear calibration curve was achieved in a concentration range of 0. 5-50 ng / m L with a lower limit of quantification of0. 5 ng / m L. The value of intra- and inter-day precision was less than 11. 3% and accuracy fell in the ranges of 94. 3%-98. 7%. The recovery ranged from 81. 3% to85. 2% and the matrix effects from 94. 3% to 103. 2%. After oral administration of ICA to rats, t1 /2was( 1. 68 ± 0. 29) h, Cmaxwas( 29. 6 ± 5. 3) ng / m L, tmaxwas( 1. 00 ± 0. 00) h, AUC0- twas( 88. 4 ± 13. 9)( h·ng) / m L.
The method is specific and accurate, suitable for preclinical pharmacokinetics of ICA.
建立超高效液相色谱 - 串联质谱（UPLC-MS / MS）法测定淫羊藿苷（ICA）的含量，并研究大鼠多次口服给药后 ICA 的药代动力学。
采用乙酸乙酯从大鼠血浆中提取 ICA 和内标物香豆雌酚（CMT），在 BEH C18（50 mm×2.1mm，1.7μm）色谱柱上，以含 0.1%（V / V）甲酸的乙腈和含 2 mmol / L 甲酸铵的水为流动相进行梯度洗脱，流速为 0.3 mL / min。在负离子电喷雾电离模式下，采用多反应监测模式，以 ICA 的 m / z 675.6→351.1、CMT 的 m / z 267.0→211.1 为母离子 - 子离子对进行定量分析。大鼠以 50 mg / kg 的多剂量口服 ICA 后采集血浆。
线性校准曲线在 0.5 - 50 ng / mL 的浓度范围内获得，定量下限为 0.5 ng / mL。日内和日间精密度值均小于 11.3%，准确度在 94.3% - 98.7%范围内。回收率在 81.3%至 85.2%之间，基质效应在 94.3%至 103.2%之间。大鼠口服 ICA 后，t1 / 2 为（1.68±0.29）h，Cmax 为（29.6±5.3）ng / mL，tmax 为（1.00±
