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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 method for the determination of triptorelin in plasma by liquid chromatography-tandem mass spectrometry (LC-MS / MS) was developed.The sample was treated with octreotide as an internal standard by using protein precipitation method.The chromatographic separation was performed on an Agilent Eclipse Plus C18RRHD (50 × 2.1 mm, 1.8 μm) The mobile phase consisted of a gradient of methanol (0.1% formic acid) -water (0.1% formic acid) .The plasma samples were preconditioned by a simple precipitation method.The octreotide was used as an internal standard.The triple quadrupole tandem mass spectrometer The results showed that the linearity of triptorelin was in the range of 0.100 ~ 30.0 ng.mL-1, the correlation coefficient r was 0.998 0. The intra-day precision (RSD) of triptorelin at the three concentrations of low, medium and high were 3.5 %, 2.2% and 3.3% respectively.The precision during the day was 1.3%, 3.0% and 3.6%, respectively.This method has good specificity, high sensitivity, easy operation, precision and accuracy to meet the testing requirements.