LC-MS/MS法测定大鼠血浆中阿魏酸的血药浓度

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。

Determination of ferulic acid in rat plasma by LC-MS/MS

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 mm) . The compound separations were detected by an API 4000 mass spectrometer equipped with a TurboIonSpray^TM 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.