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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。
Objective To establish a liquid chromatography-mass spectrometry method for the determination of valsartan in rat plasma. Methods Losartan was used as an internal standard and samples were treated with acetonitrile precipitation protein. Column: Agilent ZORBAX XDBC18 (2.1 mm × 50 mm, 5 μm), mobile phase: acetonitrile-0.1% formic acid aqueous solution, gradient elution, flow rate 0.3 mL · min -1, injection volume 1 μL, Time: 5 min. Electrospray ionization source, multiple reaction monitoring mode for positive ion detection. Investigate the specificity of the method, the standard curve and lower limit of quantification, precision and recovery, matrix effect, stability. Results Valsartan showed a good linearity (r = 0.999 0) within 10-2000 ng · m L -1 with a lower limit of quantitation of 10 ng · m L -1. The intra-day and inter-day RSDs of blood samples were 1.83% -3.83% and 5.60% -8.89%, respectively. The recoveries ranged from 78.82% to 85.98%. The samples were kept stable for 24h at room temperature, 72 hours after treatment, three times in freezing and thawing, and one month at -20 ℃. Conclusion This method is a simple, rapid and sensitive method for the determination of valsartan concentration in rat plasma, which can meet the requirements of concentration determination of low dose administration in animal experiments.