摘要
目的 建立LC-MS/MS法测定人血浆中亮菌甲素琥珀酸单酯(ASE)的方法.方法 ZorbaxSB-C18色谱柱(30 mm ×2.1 mm,3.5 μm),流动相:甲醇-20 mM乙酸铵水溶液梯度洗脱,柱温:30℃,流速:0.4 mL/min.以补骨脂甲素为内标,在负离子模式下,采用选择离子监测(SIM)方式,监测离子对分别为m/z333→233和m/z 323→221.结果 ASE LC-MS/MS法的最低检测浓度为0.5 ng/mL,在0.01 ~ 10.0μg/mL(r =0.9914)内线性关系良好.该方法下ASE日内精密度RSD分别为2.18% ~5.62%,日间精密度RSD分别为4.72% ~6.23%.方法回收率分别为93.2%~109.2%.结论 本试验建立的方法准确、快速、简便,适用于ASE体内血药浓度和生物等效性的测定.
Objective To determinate the armillarisin succinate ester (ASE)in plasma by LC-MS/MS.Methods The separation was carried out on a Zorbax SB-C18 (30 mm × 2.1 mm,3.5 μm) column and methanol -20 mM ammonium acetate aqueous as mobile phase using gradient elute at flow rate of 0.4 mL/min.Bavachin was employed as the internal standard.In negative scanning mode,quantification was performed using the transitions m/z 333→233 and m/z 323→221,respectively.Results The limits of detection was 0.5 ng/mL.The concentration of ASE showed a linear plot in the range of 0.01 ~ 10.0 μg/mL(r =0.991 4).The inter-day and intra-day relative standard deviation(RSD) for the method were 2.18% ~ 5.62% and 4.72% ~ 6.23%,respectively.The extraction recovery rate was 93.2% ~ 109.2%.Conclusion The method is proved to be accurate,sensitive and reliable.It is suitable for the determination in human plasma of ASE.
出处
《实用药物与临床》
CAS
2014年第12期1591-1593,共3页
Practical Pharmacy and Clinical Remedies
基金
湖北省自然科学基金项目(2010CDB09104)
湖北省卫生厅青年科技人才项目(QJX2012-45)
十堰市科技局2014年度引导性科研项目(14Y55
14Y59)
大学生创新训练项目(201310929003)
十堰市科技攻关项目(2013st33)