摘要
建立了液相色谱-串联质谱法测定血浆中曲普瑞林的方法.以奥曲肽为内标,采用蛋白沉淀方法进行样品处理.色谱分离使用Agilent Eclipse Plus C18RRHD(50×2.1 mm,1.8μm)色谱柱,流动相为甲醇(0.1%甲酸)-水(0.1%甲酸)梯度洗脱.血浆样品用简单的沉淀法进行预处理.奥曲肽作为内标.使用三重四级杆串联质谱仪采用正离子方式多反应检测.曲普瑞林在0.100～30.0 ng.mL-1范围内线性关系良好,相关系数r为0.998 0.方法的低、中、高3个浓度的日内精密度(RSD)分别为3.5%、2.2%和3.3%.日间精密度分别为1.3%、3.0%和3.6%.本方法专属性好、灵敏度高,操作简便,精密度和准确度均满足检测要求.
A liquid chromatography-tandem mass spectrometry method is developed for the separation and simultaneous quantification of triptorelin in rat plasma. Chromatographic separation is achieved on an Agilent Eclipse Plus C 18 RRHD （50 x 2. 1 mm, 1.8 μm）column with a mobile phase consisting of 0. 1% formic acid acetonitrile solution and 0. 1% formic acid aqueous solution by use of an efficient gradient elution. A simple precipitation methods is used to prepare the rat plasma samples. A triple quadrupole mass spectrometer is operated in positive ionization mode with multiple reaction monitoring for the detection of triptorilin. Octreotide is used as an internal standard. All calibration curves show excellent linear regressions （r = 0. 998 0） within the range of tested concentrations from 0. 100 ng . mL-1 to 30. 0 ng . mL-1. The intra-and inter-day variations are below 3.6% in terms of RSD. The method is successfully applied to the analysis of samples of triptorilin. LC/MS/MS method is rapid, efficient, and accurate for the detection of triptorilin.
出处
《烟台大学学报（自然科学与工程版）》
CAS
2012年第3期184-188,共5页
Journal of Yantai University(Natural Science and Engineering Edition)
