Zhao Min, Tao Jinhua, Qian Dawei, Liu Pei, Shang Er-xin, Jiang Shu, Guo Jianming, Su Shu-lan, Duan Jin-ao, Du Leyue
Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, Nanjing 210023, PR China.
Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, Nanjing 210023, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Jan 15;1009-1010:122-9. doi: 10.1016/j.jchromb.2015.12.020. Epub 2015 Dec 14.
A sensitive and rapid method for determination of loganin, morroniside, catalpol and acteoside in rat plasma after oral administration of Rehmannia glutinosa Libosch and Cornus officinalis Sieb drug pair based on ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS). Chromatographic separation was achieved using an Acquity UPLC BEH C18 column (100mm×2.1mm, 1.7μm) at a flow rate of 0.4mL/min, using gradient mode containing 0.1% formic acid in water and acetonitrile were used as the mobile phase A and B. Loganin, morroniside, catalpol, acteoside and the internal standard (chloramphenicol) were detected by selected reaction monitoring in the negative ion mode with the mass transition of m/z 451.0→179.0 (morroniside), m/z 435.0→227.0 (loganin), m/z 407.1→199.1 (catalpol), m/z 623.2→161.0 (acteoside) and m/z 320.8→151.9 (chloramphenicol), respectively. All calibration curves showed good linearity (r>0.991). The precision was evaluated by intra-day and inter-day assays and the RSD% were all within 9.58%. The recovery ranged from 67.62 to 80.14%. The method was successfully applied to pharmacokinetic study of the analytes in normal and doxorubicin-induced chronic kidney disease rat plasma.
基于超高效液相色谱-串联质谱法(UPLC-MS)建立一种灵敏、快速的方法,用于测定大鼠口服生地黄与山茱萸药对后血浆中马钱苷、莫诺苷、梓醇和毛蕊花糖苷的含量。采用Acquity UPLC BEH C18色谱柱(100mm×2.1mm,1.7μm),以0.4mL/min的流速进行色谱分离,采用含0.1%甲酸的水和乙腈的梯度模式作为流动相A和B。通过选择反应监测在负离子模式下检测马钱苷、莫诺苷、梓醇、毛蕊花糖苷和内标(氯霉素),其质荷比分别为m/z 451.0→179.0(莫诺苷)、m/z 435.0→227.0(马钱苷)、m/z 407.1→199.1(梓醇)、m/z 623.2→161.0(毛蕊花糖苷)和m/z 320.8→151.9(氯霉素)。所有校准曲线均显示出良好的线性(r>0.991)。通过日内和日间测定评估精密度,相对标准偏差(RSD%)均在9.58%以内。回收率在67.62%至80.14%之间。该方法成功应用于正常大鼠和阿霉素诱导的慢性肾病大鼠血浆中分析物的药代动力学研究。