Wang W, Xu J, Liu Y Y
Department of thoracic surgery, Tumor Hospital, Liaoning Province, China.
Drug Res (Stuttg). 2013 Feb;63(2):69-73. doi: 10.1055/s-0032-1331756. Epub 2013 Jan 24.
A simple LC-MS/MS method was developed for determination and pharmacokinetic study of peimine in beagle dogs. The chromatographic separation was carried out on a Agilent Zobax SB C18 column with a mobile phase consisting of acetonitrile-10 mmol/L ammonium formate (35:65, v/v) at a flow rate of 0.3 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by MRM via electro spray ionization source with positive mode. The standard curve for peimine was linear (r>0.999) over the concentration range of 1-200 ng/mL with a lower limit of quantification of 1 ng/mL. The intra- and inter-day precision (relative standard deviation) values were not higher than 15% and the accuracy (relative error) was <5% at 3 quality control levels. This simple, fast and highly sensitive method was fully validated and successfully applied to a preclinical pharmacokinetic study of peimine in dogs after oral and intravenous administration.
建立了一种简单的液相色谱-串联质谱法用于测定比格犬体内的贝母碱及其药代动力学研究。色谱分离在安捷伦Zobax SB C18柱上进行,流动相为乙腈-10 mmol/L甲酸铵(35:65,v/v),流速为0.3 mL/min。采用电喷雾电离源正模式,在三重四极杆串联质谱仪上通过多反应监测(MRM)进行检测。贝母碱的标准曲线在1-200 ng/mL浓度范围内呈线性(r>0.999),定量下限为1 ng/mL。在3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15%,准确度(相对误差)<5%。该简单、快速且高灵敏度的方法经过充分验证,并成功应用于贝母碱在犬口服和静脉给药后的临床前药代动力学研究。