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Simultaneous determination of six components of Danzhi Xiaoyao Pill in beagle plasma by HPLC-MS/MS and a study of pharmacokinetic of paeoniflorin and geniposide after single-dose administration.
Journal of Pharmaceutical and Biomedical Analysis ( IF 3.4 ) Pub Date : 2020-03-19 , DOI: 10.1016/j.jpba.2020.113269
Yong-Liang Zhu 1 , Shuang-Long Li 1 , Jun-Li Jin 1 , Jia-Ao Fang 1 , Xiang-Die Wang 1 , Ling-Yun Chen 2 , Xiang-Jun Qiu 1
Affiliation  

This study was to develop a reliable and simple high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) to detect paeoniflorin, geniposide, saikosaponin b2, liquiritin, paeonol and atractylenolide Ⅲ in beagle plasma and to study pharmacokinetic of paeoniflorin and geniposide after single-dose administration of Danzhi Xiaoyao Pill (DZXY). Chromatographic separation was performed using an Agilent C18 column, and multiple reaction monitoring (MRM) mode was used. A gradient elution procedure was used with solvent A (acetonitrile) and solvent B (0.1 % formic acid-water) as mobile phases. The elution procedure was as follows: 85 % B-30 % B (0-7 min) and 30 % B-30 % B (7.1-8 min). The flow rate was 0.3 mL/min. The column temperature was 40 ℃, and the injection volume was 10 μL. The main analytical parameters of paeoniflorin, geniposide, saikosaponin b2, liquiritin, paeonol and atractylenolide Ⅲ were m/z 525→449, m/z 433→224, m/z 780→617, m/z 417→254, m/z 167→43 and m/z 249→231, respectively. Ethyl acetate was used to extract the analytes in the plasma. Standard calibration curves of six analytes showed satisfactory linearity (r2≥0.99 2) within the determined ranges. The lower limits of quantification were 0.5 ng/mL for paeoniflorin and liquiritin, 2.5 ng/mL for geniposide and saikosaponin b2 and 1.0 ng/mL for atractylenolide Ⅲ and paeonol, respectively. The intra-day and inter-day precision (RSD %) were all below 6.94 %, and the intra-day and inter-day accuracy (RE %) were within ± 6.10 %. The recovery and ME of six analytes were 85.99 %-98.10 % and 95.78%-108.06%, respectively. Additionally, the method we established in this experiment can be successfully used to study the pharmacokinetics of paeoniflorin and geniposide in beagle plasma.

中文翻译:

HPLC-MS / MS同时测定比格犬血浆中丹脂逍遥丸的六种成分,单剂给药后pa药苷和子苷的药代动力学研究。

本研究旨在建立可靠,简单的高效液相色谱-串联质谱法(HPLC-MS / MS),以检测比格犬血浆中的eon药苷,子苷,皂苷b2,脂蛋白、,药酚和白术内酯Ⅲ,并研究study药苷和and药的药代动力学。单次服用丹芝逍遥丸(DZXY)后的gen子苷。使用Agilent C18色谱柱进行色谱分离,并使用多反应监测(MRM)模式。使用梯度洗脱程序,溶剂A(乙腈)和溶剂B(0.1%甲酸-水)作为流动相。洗脱步骤如下:85%B-30%B(0-7分钟)和30%B-30%B(7.1-8分钟)。流速为0.3mL / min。柱温为40℃,进样量为10μL。eon药苷的主要分析参数 gen子苷,皂苷b2,脂蛋白,丹皮酚和白术内酯Ⅲ为m / z 525→449,m / z 433→224,m / z 780→617,m / z 417→254,m / z 167→43和m / z分别为249→231。乙酸乙酯用于提取血浆中的分析物。在确定的范围内,六种分析物的标准校准曲线显示出令人满意的线性(r2≥0.992)。eon药苷和脂蛋白的定量下限分别为0.5 ng / mL,子苷和皂苷b2的定量下限为2.5 ng / mL,白术内酯Ⅲ和丹皮酚的定量下限分别为1.0 ng / mL。日内和日间精度(RSD%)均低于6.94%,日间和日间精度(RE%)均在±6.10%以内。六种分析物的回收率和ME分别为85.99%-98.10%和95.78%-108.06%。另外,
更新日期:2020-03-20
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