School of Chemistry and Chemical Engineering, Guangxi University, Nanning, China.
State Key Laboratory of Conservation and Utilization of Subtropical Agro-bioresources, Guangxi University, Nanning, China.
Biomed Chromatogr. 2021 Feb;35(2):e4975. doi: 10.1002/bmc.4975. Epub 2020 Sep 15.
A rapid and sensitive ultrahigh-performance liquid chromatography-tandem mass spectrometry method was developed and validated for simultaneous determination of 15 bioactive ingredients in rat plasma and tissues after oral administration of Polygonum chinense Linn extract (PCE). After addition of internal standards (ISs; rutin and danshensu), plasma and tissue samples were pre-treated by protein precipitation with acetonitrile-ethanol. The chromatographic separation was performed on an Agilent ZORBAX RRHD Eclipse Plus C column with gradient elution using a mobile phase composed of methanol and water (containing 0.2% acetic acid) at a flow rate of 0.3 mL min . Mass spectrometric detection was carried out using a mass spectrometer in both positive and negative ion electrospray ionization modes by multiple reaction monitoring. The method provided excellent linearity, and the lower limit of quantification range 0.5-30 ng mL for all analytes. The intra- and inter-day precision were less than 9.12% and the accuracy ranged from -4.02% to 6.32%, respectively. The mean extraction recovery and matrix effect of analytes and ISs ranged from 83.65% to 109.20%. The method was successfully applied to the pharmacokinetics and tissue distribution study of 15 ingredients of PCE in rats.
建立并验证了一种灵敏、快速的超高效液相色谱-串联质谱法，用于测定口服Polygonum chinense Linn 提取物（PCE）后大鼠血浆和组织中 15 种生物活性成分的含量。加入内标（芦丁和丹参素）后，采用乙腈-乙醇沉淀蛋白法预处理血浆和组织样品。采用 Agilent ZORBAX RRHD Eclipse Plus C 柱，以甲醇和水（含 0.2%乙酸）为流动相，梯度洗脱，流速为 0.3ml/min，进行色谱分离。质谱检测采用正、负离子电喷雾电离模式，多重反应监测。该方法具有良好的线性，所有分析物的定量下限范围为 0.5-30ng/ml。日内和日间精密度均小于 9.12%，准确度在-4.02%至 6.32%之间。分析物和内标的平均提取回收率和基质效应在 83.65%至 109.20%之间。该方法成功应用于大鼠体内 PCE 的 15 种成分的药代动力学和组织分布研究。
