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目的建立银荷方药物制备物及大鼠血浆中槲皮素、山奈酚、异鼠李素的含量测定方法,以研究银荷方药物制备物黄酮类成分的质量表征特性。方法制备物和血浆样品均加酸进行水解,并用乙醚-丙酮(14∶1)萃取法处理血浆样品,采用HPLC分析,以C_(18)为固定相,流动相为乙腈-0.2%磷酸水溶液梯度洗脱,在270 nm检测黄酮类苷元槲皮素、山奈酚、异鼠李素的含量。结果经方法学考证,槲皮素、山奈酚、异鼠李素的线性范围分别为1.49~29.70 mg/L(r=0.999 3),0.65~12.90mg/L(r=0.999 5),0.47~9.40 mg/L(r=0.999 0),日内、日间精密度RSD≤5.85%,血浆样品冻融稳定性良好,室温放置10 h,在-80℃条件下保存1个月的稳定性均良好,符合生物样品分析要求。槲皮素、山奈酚、异鼠李素在正常组中的血药浓度分别为7.25、1.71、3.73 mg/L,在血栓组中血药浓度分别为8.53、2.64、5.69 mg/L,在抗凝组中血药浓度分别为8.32、2.76、4.56 mg/L。结论本文所建立的检测方法适用于银荷方药物制备物黄酮类成分槲皮素、山奈酚和异鼠李素的体内含量测定,并可应用于分析黄酮类成分质量表征特性,为基于黄酮类成分的银荷方药物质量精准控制提供科学依据。
OBJECTIVE To establish a method for the determination of quercetin, kaempferol and isorhamnetin in plasma of Yin Hefang and rat plasma, in order to study the quality characterization of flavonoids in Yin Hefang prescription. Method preparations and plasma samples were hydrolyzed by acid, and plasma samples were extracted by ether-acetone (14: 1) extraction method. HPLC analysis showed C_ (18) as the stationary phase and the mobile phase consisted of acetonitrile-0.2% Elution, at 270 nm flavonoid glycosides quercetin, kaempferol, isorhamnetin content. Results The linear range of quercetin, kaempferol and isorhamnetin were 1.49 ~ 29.70 mg / L (r = 0.999 3), 0.65 ~ 12.90 mg / L (r = 0.999 5) 9.40 mg / L (r = 0.999 0). The intra-day and inter-day precision RSD was less than or equal to 5.85%. The stability of plasma samples was good at freezing and thawing. After being stored at room temperature for 10 hours, the stability of the samples stored at -80 ℃ for 1 month was good , In line with biological sample analysis requirements. Quercetin, kaempferol, isorhamnetin in the normal group, the plasma concentrations were 7.25,1.71,3.73 mg / L, respectively, in the thrombus group were 8.53,2.64,5.69 mg / L plasma concentration, in the anti- The plasma concentration of coagulation group were 8.32,2.76,4.56 mg / L respectively. Conclusion The detection method established in this paper is suitable for the determination of flavonoids quercetin, kaempferol and isorhamnetin in Yin Hefang, and can be used to analyze the quality characterization of flavonoids. The composition of the Silver Dutch side of the drug quality control to provide a scientific basis.