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目的:建立同时测定大鼠灌服双黄连制剂后血浆中酚酸类(新绿原酸、绿原酸及隐绿原酸)与黄酮类(黄芩苷、千层纸素A-7-O-β-D-葡萄糖苷、汉黄芩苷、黄芩素、汉黄芩素及千层纸素A)成分的超高效液相色谱-串联质谱法(UPLC-MS/MS),并研究其药代动力学。方法:血浆样品采用乙酸乙酯-正丁醇(1∶1)萃取,流动相0.4%甲酸水溶液-[乙腈-甲醇(4∶1)混合液]梯度洗脱,流速0.4 m L·min-1,采用电喷雾离子化,多反应监测离子扫描模式,选用响应较高的正离子模式。结果:建立的同时测定血浆中9种成分的UPLC-MS/MS线性良好(R2>0.992),精密度RSD均<14.2%,准确度85.49%~114.76%,复方中新绿原酸、绿原酸、隐绿原酸、黄芩苷、千层纸素A-7-O-β-D-葡萄糖苷、汉黄芩苷、黄芩素的药时曲线下面积AUC0-t与AUC0-∞与单味药提取物相比显著增加,而酚酸和黄酮类成分的消除速率较单味药提取液缓慢。结论:建立的UPLC-MS/MS特异、快速、准确及灵敏,可用于双黄连制剂中9种主要活性成分在大鼠体内的药代动力学研究。
OBJECTIVE: To establish a method for the simultaneous determination of plasma concentrations of phenolic acids (neogenic chlorogenic acid, chlorogenic acid and chlorogenic acid) and flavonoids (baicalin, melatonin A-7-O-β (UPLC-MS / MS) was developed and its pharmacokinetics were studied by HPLC-MS. METHODS: The plasma samples were extracted with ethyl acetate-n-butanol (1: 1) and the mobile phase was eluted with a gradient of 0.4% formic acid in water and acetonitrile / methanol , Using electrospray ionization, multi-reaction monitoring ion scan mode, the choice of higher positive ion mode. Results: The established UPLC-MS / MS with good linearities (R2> 0.992) showed that the RSDs were all <14.2% and the accuracy was 85.49% ~ 114.76% , The area under the curve of AUC0-t and AUC0-∞ of the hidden-chlorogenic acid, baicalin, meyerin A-7-O-β-D-glucoside, baicalin and baicalein, Compared with the single drug extract, the elimination rate of phenolic acids and flavonoids was slow. CONCLUSION: The established UPLC-MS / MS is specific, rapid, accurate and sensitive and can be used to study the pharmacokinetics of nine major active ingredients in Shuanghuanglian formulations in rats.