LC-MS/MS法测定大鼠血浆中阿魏酸的血药浓度Determination of ferulic acid in rat plasma by LC-MS/MS
吴瑞阳,金艺,刘晓红,甘晶晶,徐海燕,袁波
WU Rui-yang,JIN Yi,LIU Xiao-hong,GAN Jing-jing,XU Hai-yan,YUAN Bo*(School of Pharmacy
摘要(Abstract):
目的建立高效液相色谱-串联质谱(LC-MS/MS)法测定大鼠血浆中阿魏酸的血药质量浓度。方法色谱柱采用Diamonsil C18柱(150 mm×4.6 mm,5μm),仪器采用API 4000三重四极杆串联质谱仪,采用多反应监测(multiple reaction monitoring,MRM)扫描方式检测,采用沉淀蛋白法处理样品,用于定量分析的离子对为m/z 193.1→m/z 134.1(阿魏酸)和m/z 121.2→m/z 77.0(苯甲酸,内标)。结果该方法的线性范围在5.0~2 000.0μg.L-1,定量下限为5.0μg.L-1,且血浆中内源性物质不干扰阿魏酸的测定;日内和日间精密度RSD均小于15%;阿魏酸的平均提取回收率为91.0%~100.5%,基质效应在87.8%~89.7%。结论该方法适用于阿魏酸在大鼠体内的药物动力学研究。
Objective To develop a simple,rapid and sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the determination of ferulic acid in rat plasma.Methods Protein precipitation was used for the sample pretreatment with a plasma volume of 50 μL.The chromatographic separation was carried out on an Diamonsil C18 analytical column(150 mm×4.6 mm,5 μm).The compound separations were detected by an API 4000 mass spectrometer equipped with a TurboIonSprayTM interface.The compounds were quantified by multiple-reaction monitoring(MRM) mode using the transition mass of m/z 193.1→m/z 134.1 for ferulic acid and m/z 121.2→m/z 77.0 for benzoic acid.Results The method was linear over the range of 5.0-2 000.0 μg · L-1 and the lower limit of quantification(LLOQ) was 5.0 μg · L-1.The intra-and inter-day precision was within 15.0% in terms of relative standard deviation(RSD%).The average recoveries were between 91.0-100.5%,the matrix effects were between 87.8-89.7%.Conclusions This simple and sensitive LC-MS/MS method is successfully applied to pharmacokinetic studies of ferulic acid in SD rats after oral administration of 10 mg · kg-1 ferulic acid.
关键词(KeyWords):
阿魏酸;液-质连用;药物动力学
ferulic acid;LC-MS/MS;pharmacokinetics
基金项目(Foundation): 国家自然科学基金资助项目(30901996)
作者(Author):
吴瑞阳,金艺,刘晓红,甘晶晶,徐海燕,袁波
WU Rui-yang,JIN Yi,LIU Xiao-hong,GAN Jing-jing,XU Hai-yan,YUAN Bo*(School of Pharmacy
DOI: 10.14066/j.cnki.cn21-1349/r.2013.08.012
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