Wei Xiao-Yan, Tao Jin-Hua, Cui Xiang, Jiang Shu, Qian Da-Wei, Duan Jin-Ao
Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, 138 Xianlin Road, Nanjing 210023, PR China.
School of Pharmacy, Nantong University, Nantong 226001, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:248-255. doi: 10.1016/j.jchromb.2017.07.026. Epub 2017 Jul 17.
A rapid, sensitive, and selective UPLC-TQ-MS/MS method was established and validated for the determination and pharmacokinetic investigation of rhein, coptisine, berberine, palmatine, baicalin and wogonoside from Sanhuang Xiexin Decoction (SXD) extracts. A Waters BEH C UPLC column was used with the mobile phases of Acetonitrile-0.1% formic acid-water. The lower limits of quantification (LLOQ) for rhein, coptisine, berberine, palmatine, baicalin and wogonoside were 24.16, 0.72, 0.68, 0.53, 18.07 and 28.56ng/mL, respectively. All calibration curves displayed good linearity (r>0.995). The precision was evaluated by intra-day and inter-day assays and the RSD% were all within 9.12%, and the bias of the accuracies ranged from -7.50% to 8.03%. The recovery ranged from 74.83% to 94.32% and the matrix effects of six analytes were found to be between 90.17% and 103.10%. The stability study showed that compounds were stable during the experiment. Finally, the data showed that the pharmacokinetic (PK) profiles (especially AUC, Tmax and Cmax) of six analytes in diabetic rats were significantly diverse from that in normal group rats. The PK study under the pathological condition could provide more helpful information to guide the clinical usage of SXD to treat T2DM.
建立并验证了一种快速、灵敏且具选择性的超高效液相色谱-串联质谱(UPLC-TQ-MS/MS)方法,用于测定三黄泻心汤(SXD)提取物中的大黄酸、黄连碱、小檗碱、巴马汀、黄芩苷和汉黄芩苷,并进行药代动力学研究。采用沃特世BEH C18超高效液相色谱柱,以乙腈-0.1%甲酸-水为流动相。大黄酸、黄连碱、小檗碱、巴马汀、黄芩苷和汉黄芩苷的定量下限(LLOQ)分别为24.16、0.72、0.68、0.53、18.07和28.56 ng/mL。所有校准曲线均显示出良好的线性(r>0.995)。通过日内和日间测定评估精密度,相对标准偏差(RSD%)均在9.12%以内,准确度偏差范围为-7.50%至8.03%。回收率范围为74.83%至94.32%,六种分析物的基质效应在90.17%至103.10%之间。稳定性研究表明,化合物在实验过程中稳定。最后,数据表明糖尿病大鼠体内六种分析物的药代动力学(PK)曲线(尤其是AUC、Tmax和Cmax)与正常组大鼠有显著差异。病理条件下的PK研究可为指导SXD治疗2型糖尿病的临床应用提供更有用的信息。