Li H, Wen X-S, Di W
Department of Chinese Traditional Medicine, Renji Hospital Jiaotong University School of Medicine, Shanghai, China.
Arzneimittelforschung. 2012 Feb;62(2):83-7. doi: 10.1055/s-0031-1295485. Epub 2012 Feb 16.
A simple LC-MS/MS method was developed for determination and pharmacokinetic study of magnolol in rat blood. Blood sample pretreatment involved a one-step extraction with methanol of 100 µL blood. The chromatographic separation was carried out on a Agilent Zobax SB C18 column with a mobile phase consisting of acetonitrile-0.2% formic acid (55:45, v/v) at a flow rate of 0.3 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via electro spray ionization source with positive mode. A high throughput was achieved with a run time of 4 min per sample. The standard curve for magnolol was linear (r > 0.999) over the concentration range of 2-1 000 ng/mL, with a lower limit of quantification of 2 ng/mL. The intra- and inter-day precision (relative standard deviation) values were not higher than 12% and the accuracy (relative error) was <5% at three quality control levels. This simple, fast and highly sensitive method was fully validated and successfully applied to a clinical pharmacokinetic study of magnolol in rats after oral administration.
建立了一种简单的液相色谱-串联质谱法用于大鼠血液中厚朴酚的测定及药代动力学研究。血样预处理采用用甲醇对100 μL血液进行一步萃取的方法。色谱分离在安捷伦Zobax SB C18柱上进行，流动相为乙腈-0.2%甲酸（55:45，v/v），流速为0.3 mL/min。检测在三重四极杆串联质谱仪上进行，通过电喷雾电离源以正模式进行多反应监测。每个样品的运行时间为4分钟，实现了高通量。厚朴酚的标准曲线在2-1000 ng/mL的浓度范围内呈线性（r>0.999），定量下限为2 ng/mL。在三个质量控制水平下，日内和日间精密度（相对标准偏差）值不高于12%，准确度（相对误差）<5%。这种简单、快速且高度灵敏的方法经过了充分验证，并成功应用于厚朴酚口服给药后大鼠的临床药代动力学研究。
