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作 者:吴云[1] 艾玉[1] 王粉绒 马文[1] 边巧侠 戴荣华[1]
出 处:《沈阳药科大学学报》2016年第5期396-401,共6页Journal of Shenyang Pharmaceutical University
基 金:国家自然科学基金资助项目(81373924)
摘 要:目的建立测定阿魏酸在大鼠血浆中质量浓度的超高效液相色谱-串联质谱(UPLC-MS/MS)法,并将该方法用于分别灌胃给予活络效灵丹、川芎提取物及当归提取物后正常大鼠及佐剂性关节炎大鼠体内阿魏酸的比较药动学研究。方法色谱柱为Shim-pack XR-ODS(75 mm×3.0 mm,2.2μm)柱,血浆样品酸化后经液-液萃取处理,流动相为甲醇-水(含体积分数0.1%甲酸溶液)(体积比30∶70),负离子检测模式,扫描方式为多反应监测(multiple reaction monitoring,MRM)。结果阿魏酸在质量浓度2.5~1 250μg·L-1内线性关系良好,定量下限为2.5μg·L-1,日内和日间精密度(RSD)均〈15%,准确度(RE)在±15%以内,阿魏酸的平均提取回收率在88.6%~93.0%内,基质效应为86.4%~105.6%。结论该方法适用于阿魏酸在大鼠体内的比较药动学。Objective To develop a simple and sensitive ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS / MS) method for the determination of ferulic acid in rat plasma,and apply this method to the comparative pharmacokinetic study of ferulic acid between normal and arthritic rats after oral administration of Huo Luo Xiao Ling Dan,Ligusticum chuanxiong extract and Angelica sinensis extract,respectively. Methods After liquid-liquid extraction,chromatographic separation was accomplished on a Shim-pack XR-ODS column( 75 mm × 3. 0 mm,2. 2 μm) with the mobile phase consisting of methanol-0. 1%( φ) formic acid in water( V ∶ V = 30∶ 70). A triple quadrupole tandem mass spectrometry equipped with an electrospray ionization source was used as detector operated in negative ionization mode and by multiplereaction monitoring scanning. Results A linear relationship of ferulic acid ranged from 2. 5 to1 250 μg·L- 1,and the lower limit of quantification was 2. 5 μg·L- 1. Both intra-day and inter-day precision and accuracy were well within acceptance criteria( ± 15%). The mean recoveries of ferulic acid were between 88. 6%- 93. 0% and the matrix effects were between 86. 4%- 105. 6%. Conclusions The UPLCMS / MS method is suitable for the comparative pharmacokinetic study of ferulic acid in rat plasma.
关 键 词:阿魏酸 活络效灵丹 川芎 当归 超高效液相色谱-串联质谱 药动学
分 类 号:R917[医药卫生—药物分析学]
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