摘要
目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定大鼠血浆中桑色素的含量,并对其在大鼠体内的药动学特征进行研究。方法以芫花素为内标,血浆样品经乙腈沉淀蛋白后,采用Thermo Hypersil GOLD-C18(50mm×4.6mm,3μm)色谱柱进行梯度洗脱,流动相为0.1%甲酸水溶液(A)-乙腈(B),进样量2μl,柱温40℃,流速0.5ml/min。质谱采用电喷雾离子源(ESI),负离子模式,以多反应监测模式(MRM)检测。桑色素和内标的定量离子对分别为m/z300.9→151.2和283.1→268.2。结果桑色素的浓度在1.01~504.2ng/ml范围内线性良好(r2≥0.99);定量下限为1.01ng/ml;精密度、准确度、回收率、基质效应和稳定性均符合生物样品的分析要求。结论本方法可满足大鼠血浆中桑色素的测定及药动学研究的要求。
Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLCMS/ MS) method for determination of morin in plasma of rats and study its pharmacokinetic properties. Methods Genkwanin was used as internal standard (IS). Plasma samples were pretreated via protein precipitation with acetonitrile, then were separated on a Thermo Hypersil GOLD C18 column (50 mm×4.6 mm, 3 μm). Gradient elution was performed, using acetonitrile-0.1 % formic acid in water at the flow rate of 0.5 ml/min as mobile phase. The temperature of column was set at 40 ℃. The injection volume was 2 μl. MS was operated with a negative electrospray ionization (ESI) source and scanned with multipe-reaction monitoring (MRM) mode. The transitions of m/z 300.9→151.2 for morin and m/z 283.1→268.2 for IS were chosen for quantification. Results The concentration of morin was linear within the range of 1.01-504.2 ng/ml (r2≥0.99). The lower limit of quantification (LLOQ) was 1.01 ng/ml. Precision, accuracy, recovery, matrix effect and stability all met the analytical requirements of analysis of biological samples. Conclusion The method can meet the requirements of determination of morin in plasma of rats as well as its pharmacokinetic study.
作者
柳佳
姚庆强
邓志鹏
LIU Jia;YAO Qing-qiang;DENG Zhi-peng(School of Medicine and Life Sciences, University of Jinan-Shandong Academy of Medical Sciences, Jinan 250200,China;Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, China;Key Laboratory for Biotech Drugs, Ministry of Health, Jinan 250062, China;Key Laboratory for Rare & Uncommon Diseases of Shandong Province, Jinan 250062, China)
出处
《食品与药品》
CAS
2019年第5期342-346,共5页
Food and Drug
基金
山东省自然科学基金-面上项目（编号：ZR2019MH051）
关键词
超高效液相色谱-串联质谱法
桑色素
药动学
ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
morin
pharmacokinetics
