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本研究建立并验证了一种快速且灵敏的液质联用方法,用于测定小鼠血浆和脑组织中沙奎那韦的浓度,并将其应用于初步筛选实验,以评价黄酮类化合物对沙奎那韦脑内分布影响的作用。血浆和脑组织中的沙奎那韦和内标利托那韦通过液-液萃取的方式进行提取,色谱分离过程使用C18反相色谱柱(150 mm×2.1 mm,5.0μm)。质谱检测过程使用三重四极杆串联质谱,以电喷雾正离子模式、质谱多反应监测技术对沙奎那韦和内标进行检测。血浆中测定标准曲线的线性范围为0.1至10 ng/m L,其最低浓度为定量下限。方法日间日内精密度为7.5%–12.1%,准确度介于90.5%与107.2%之间。脑组织中测定标准曲线的线性范围为0.1至10 ng/g,其最低浓度为定量下限。方法日间日内精密度为7.3%–11.9%,准确度介于90.8%与107.4%之间。该方法成功应用于初步筛选实验,评价了19种黄酮类化合物对沙奎那韦脑内分布影响的作用,结果显示biochanin A能够最大程度促进沙奎那韦的脑内分布。
This study established and validated a rapid and sensitive LC-MS method for the determination of the concentration of saquinavir in mouse plasma and brain tissue and applied it to preliminary screening experiments to evaluate the effect of flavonoid pairs Effects of saquinavir intracerebral distribution. Saquinavir in plasma and brain and endolitidine internal standard were extracted by liquid-liquid extraction using a C18 reversed-phase column (150 mm × 2.1 mm, 5.0 μm). Mass spectrometry detection process using triple quadrupole tandem mass spectrometry, electrospray positive ion mode, mass spectrometry multiple reaction monitoring of saquinavir and internal standard detection. The calibration curve in plasma has a linear range of 0.1 to 10 ng / mL, with the lowest concentration being the lower limit of quantitation. Methods Intra-day precision was 7.5% -12.1% with an accuracy of between 90.5% and 107.2%. The linearity of the standard curve in brain tissue was determined to be 0.1 to 10 ng / g, with the lowest concentration being the lower limit of quantitation. Methods Intra-day precision was 7.3% -11.9% with an accuracy of between 90.8% and 107.4%. This method was successfully applied to preliminary screening experiments to evaluate the effect of 19 flavonoids on the brain distribution of saquinavir. The results showed that biochanin A can maximize the brain distribution of saquinavir.