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目的建立同时测定比格犬血浆中美托拉宗和缬沙坦的高效液相色谱串联质谱法。方法分析柱为Agilent Poroshell 120色谱柱(2.1 mm×30 mm×2.7μm)。质谱采用电喷雾离子源(ESI),采用多反应监测(MRM),检测离子为正离子,分别选择m/z 366.2/259、436.2/291和423.4/207作为美托拉宗、缬沙坦和内标(氯沙坦钾)的检测离子对。结果美托拉宗、缬沙坦的线性范围分别为0.5~100及5~5000 ng/ml,相关系数r2分别为0.9937和0.9939,批内精密度分别为2.09%~8.85%和2.36%~13.12%,基质效应分别为87.73%~98.62%和99.03%~137.35%,回收率分别为75.74%~81.82%和83.89%~95.64%。结论该法操作简单、准确可靠、检测灵敏度高,可用于复方美托拉宗缬沙坦速释片比格犬体内的药代动力学研究。
OBJECTIVE To establish simultaneous high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the simultaneous determination of memantonate and valsartan in beagle dogs plasma. Method The analytical column was an Agilent Poroshell 120 column (2.1 mm × 30 mm × 2.7 μm). Mass spectrometry was performed on electrospray ionization source (ESI). Multiple reaction monitoring (MRM) and positive ions were used as positive ions. The m / z 366.2 / 259,436.2 / 291 and 423.4 / Internal standard (losartan potassium) detection of ion pairs. Results The linear ranges of metolazone and valsartan were 0.5-100 and 5-5000 ng / ml, respectively. The correlation coefficients r2 were 0.9937 and 0.9939 respectively. The intra-assay precision was 2.09% -8.85% and 2.36% -13.12, respectively The matrix effects were 87.73% ~ 98.62% and 99.03% ~ 137.35%, respectively. The recoveries were 75.74% ~ 81.82% and 83.89% ~ 95.64%, respectively. Conclusion The method is simple, accurate and reliable, and has high detection sensitivity. It can be used to study the pharmacokinetics of compound MTX valsartan immediate release tablets in beagle dogs.