液质联用法检测大鼠血浆中缬沙坦的浓度

发布时间：2018-03-24 00:40

  本文选题：缬沙坦　切入点：氯沙坦　出处：《中国临床药理学杂志》2016年10期

【摘要】：目的建立检测大鼠血浆中缬沙坦浓度的液质联用方法。方法选择氯沙坦作为内标,用乙腈沉淀蛋白法处理样本。色谱柱:Agilent ZORBAX XDBC18(2.1 mm×50 mm,5μm),流动相:乙腈-0.1%甲酸水溶液,梯度洗脱,流速:0.3 m L·min~(-1),进样量:1μL,分析时间:5 min。用电喷雾离子源,多反应监测模式进行正离子检测。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应、稳定性。结果缬沙坦在10~2000 ng·m L~(-1)内线性关系良好(r=0.999 0),定量下限为10 ng·m L~(-1)。血样日内及日间RSD分别为1.83%~3.83%和5.60%~8.89%,回收率为78.82%~85.98%。室温放置24h、处理后放置72 h、冻融3次及-20℃冻存1个月后样本均保持稳定。结论本方法是一种简单、快速、灵敏的检测大鼠血浆中缬沙坦浓度的方法,可满足动物实验中低剂量给药的浓度测定要求。
[Abstract]:Objective to establish a HPLC method for the determination of valsartan in rat plasma. Methods Losartan was selected as internal standard and the sample was treated with acetonitrile precipitation protein method. The mobile phase consisted of acetonitrile-0.1% formic acid solution and gradient elution. The velocity of flow is 0.3 mL / L, the injection amount is 1 渭 L, and the analysis time is 1: 5 min. The positive ion is detected by electrospray ion source and multi-reaction monitoring mode. The specificity, standard curve and quantification limit, precision and recovery rate, matrix effect of the method are investigated. Results the linear relationship of valsartan was good in 10 ~ 2 000 ng / L ~ (-1). The lower limit of quantification was 10 ng / m ~ (L ~ (-1)). The RSD of blood samples was 1.83% and 5.60% respectively. The recovery rate was 78.822 ~ 85.98. At room temperature for 24 h, after treatment for 72 h, freezing and thawing for 3 times and freezing at -20 鈩，

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