【作者】 唐跃年； 金樑； 张健； 陆晓彤；

【Author】 Tang Yuenian, Jin Lian,Zhang Jian, Lu Xiaotong (Department of Pharmacy, Xin-Hua hospital Affiliated Shanghai Jiao Tong University Medical School, Shanghai 200092)

【机构】 上海交通大学医学院附属新华医院药剂科；

【摘要】 建立了同时检测射干合剂样品中黄芩苷等5种黄酮类化合物含量的反相高效液相色谱法。样品经超声提取后,用InertsilODS-3色谱柱分离样品,流动相为乙腈/1‰磷酸(pH=2.25),梯度洗脱,流量为1mL.min-1,柱温为室温,用紫外检测仪260nm测定;外标法定量。对于待测组分γ均大于0.999;黄芩苷、黄芩素、汉黄芩素、射干苷、次野鸢尾黄素的线性范围分别为50ng.mL-1-10000ng.mL-1、50ng.mL-1-1000ng.mL-1、50ng.mL-1-1000ng.mL-1、50ng.mL-1-1000ng.mL-1、50ng.mL-1-1000ng.mL-1;检出限为10-20ng.mL-1。方法加样回收率为94.5-103.2%;相对标准偏差(RSD)低于4.7%(n=3)。可用于射干合剂中黄酮类化合物多指标成分的含量测定,方法简便、准确、灵敏度高,也可用于制剂及体内指标成分的研究。更多还原

【Abstract】 A method was developed for the determination of baicalin and selected flavonoids in Shegan mixture by reversed phase high performance liquid chromatography. Shegan mixture samples were extracted with selective ultrasound extraction. Separation and quantifica-tion were achieved by a InertsilODS-3 column under the optimum conditions: Acetonitrile-1‰ phosphoric acid aqueons (2/3,V/V,pH=2.25)as mobile phase at a flow rate of l ml /min, at room temperature and detected with UV detector at 260nm.The quantified analysis of external standard calibration curves was used·The calibration graph was linear in the ranger of 50-10 000、50-1 000、50-1 000、50-1 000、50-1 000 ng.mL-1; with r>0.999 for BCL、BCN、 WGN、TRD、IRT,respectively. Limits of detection varied from l0 to 20 ng.mL-1.For spiked plasma analysis,the RSD was less than 4.7% and there coveries were 94.5%-103.2%. This method is simple,accurate and convenient,and can be applied to the Shegan mixture samples from interventional studies as well as observational studies.更多还原