摘要
目的建立一种检测兔血浆中利格列汀浓度的超高效液相色谱-串联质谱(UPLC-MS/MS)的方法。方法以地西泮为内标,血浆样品用乙腈沉淀后检测。用Acquity UPLC BEH C18柱为分离柱,流动相:乙腈-0.1%甲酸梯度洗脱,总运行时间为3.0 min,利格列汀的洗脱时间为1.09 min;用AcquityXevo TQD三重四级杆质谱仪检测,用多反应监测法测定样品中的药物浓度。考察该方法的专属性、线性关系、精密度、准确度和回收率及稳定性。结果色谱图显示血浆中的利格列汀保留时间为1.09 min,无内生峰干扰;校准曲线的典型方程:y=0.1646x+0.0303,r=0.9914,线性关系良好;日内、日间精密度及准确度范围均低于15%;药物回收率在76.0%~82.1%范围内;在不同储存条件下浓度的偏差在均值的±15%以内,较稳定。结论该方法简便、快速,可用于兔血浆利格列汀的检测、药代动力学研究和药物相互作用研究。
Objective To establish a method for the determination of linagliptin in rabbit plasma by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods After the rabbit plasma samples were precipitated with acetonitrile,diazepam was used as the internal standard for the determination of linagliptin.Acquity UPLC BEH C18 column was used as the separation column.The gradient elution of linagliptin was performed using a mobile phase of acetonitrile-0.1%formic acid.The total running time was 3.0 min,and the eluting time of linagliptin was 1.09 min.Acquity Xevo TQD triple quadrupole mass spectrometer was used for detection.The concentration of the drug in the samples was determined by multiple reaction monitoring(MRM).The specificity,linearity,precision,accuracy,recovery and stability of the method were investigated.Results The chromatogram showed that the retention time of linagliptin in plasma was 1.09 min,without the interference of endogenous peaks.The typical equation of the calibration curve was(y=0.1646x+0.0303,r=0.9914),with a good linear relationship.The within-day and between-day precisions and accuracies were less than 15%.The drug recovery rate was in the range of 76.0%~82.1%.The deviation of the drug concentrations under different storage conditions was within±15%of the mean value,which was relatively stable.Conclusion The method is simple and can be used for rapid determination of linagliptin in rabbit plasma,pharmacokinetic research and drug interaction study.
作者
郑孝振
刘静
李明明
任益锋
韩箫笛
ZHENG Xiao-zhen;LIU Jing;LI Ming-ming(Department of Anesthesia and Perioperative Medicine, the First Affiliated Hospital of Henan University, Kaifeng 475000, China)
出处
《中国临床新医学》
2020年第12期1221-1225,共5页
CHINESE JOURNAL OF NEW CLINICAL MEDICINE
基金
河南省科技发展计划项目(编号:192102310367)
开封市科技发展计划项目(编号:1803028)。
关键词
超高效液相色谱-串联质谱法
利格列汀
兔血浆
含量测定
药代动力学
Ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
Linagliptin
Rabbit plasma
Content determination
Pharmacokinetics
