摘要
目的建立超高效液相色谱-串联质谱法测定大鼠血浆中辛夷脂素,并对辛夷脂素大鼠口服(15 mg/kg)的药代动力学进行研究。方法以白当归脑为内标,采用UPLC BEH C18(2.1 mm×50 mm, 1.7μm)柱,流动相由乙腈和0.1%甲酸组成,梯度洗脱流速为0.4 ml/min。MRM模式对辛夷脂素m/z 371.0→353.2和内标m/z 317.0→233.1进行定量分析。乙腈沉淀法去除蛋白处理大鼠血浆样本。验证方法按照美国食品药品监督管理局(FDA)生物分析方法验证指南进行。验证项目包括选择性、基质效应、线性、精密度、准确度、回收率和稳定性。结果在1 ng/ml^1 000 ng/ml浓度时,大鼠血浆中辛夷脂素线性良好(r>0.995),最低定量下限为1 ng/ml。大鼠血浆中辛夷脂素日内精密度RSD<11%,日间精密度RSD<12%,准确度在90.1%~108.9%,平均回收率高于88.9%,基质效应在100.8%~108.6%。结论该分析方法灵敏、快速、选择性好,并成功应用于辛夷脂素大鼠药代动力学研究。
Objective In this work, the UPLC-MS/MS method was used for the determination of fargesin in rat plasma, and the pharmacokinetics of fargesin rats after orally were studied. Methods Byakangelicol was used as the internal standard, UPLC BEH C18(2.1 mm×50 mm, 1.7 μm) column was used. The mobile phase consisted of acetonitrile and 0.1% formic acid at a flow of 0.4 ml/min. The rat plasma samples were treated by acetonitrile precipitation. Multiple reaction monitoring was used for quantitative analysis, m/z 371.0→353.2 for fargesin and m/z 317.0→233.1 for byakangelicol. The verification method was established in accordance with the US Food and Drug Administration(FDA) bioanalytical method validation guidelines. Validation projects included selectivity, matrix effects, linearity, precision, accuracy, recovery, and stability. Results In the range of 1 ng/ml-1 000 ng/ml, fargesin in rat plasma was linear(r > 0.995), and the lowest quantitative lower limit was 1 ng/ml. The intra-day and inter-day precision of fargesin were less than 11% and 12%, respectively. The accuracy ranged from 90.1% to 108.9%. The recovery was higher than 88.9%. The matrix effect was within 100.8%-108.6%.Conclusion The method was sensitive, fast, specific, and has been successfully applied to a pharmacokinetic study of fargesin after oral administration.
作者
孙文浩
鲍曦
林崇良
SUN Wen-hao;BAO Xi;LIN Chong-liang(Department of Pharmacy,the First Affiliated Hospital of Hangzhou Normal University,Hangzhou,Zhejiang 310000,China)
出处
《中国卫生检验杂志》
CAS
2019年第16期1932-1934,1941,共4页
Chinese Journal of Health Laboratory Technology
基金
温州市公益性科技计划项目(Y20140236)
