Wang Zilingyun, An Rui, Du Guangli, Liang Kun, Li Guowen
Shanghai University of Traditional Chinese Medicine, Shanghai, China.
Shanghai Hospital of Integrated Traditional Chinese and Western Medicine, Affiliated to Shanghai University of Traditional Chinese Medicine, Shanghai, China.
Biomed Chromatogr. 2019 Jul;33(7):e4524. doi: 10.1002/bmc.4524. Epub 2019 Mar 21.
A sensitive and validated method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established to test the plasma concentrations of active ingredients in Qinxing Qingre Zhike Granule, namely geniposide, liquiritin, isoliquiritin, baicalin, wogonoside, baicalein, liquiritigenin, isoliquiritigenin and glycyrrhetinic acid. The analysis was performed on an Ultimate XB-C column at the flow rate of 0.4 mL min in a single run of 18 min. The mobile phase was composed of 0.05% formic acid in water and acetonitrile with gradient elution. Positive and negative scanning and selected multiple reaction monitoring modes were applied for quantization. The proposed method showed good linearity in the given ranges from 0.6800-340.0 to 3.920-1960 ng mL with r > 0.9917 for all the analytes. The precision (RSD) was no more than 12%, and the accuracy (RE) was less than ±11% for intra- and inter-day. The extract recovery and matrix effect were acceptable for the requirements of biological sample analysis. Moreover, the developed method was effectively applied to the pharmacokinetic investigation of Qinxing Qingre Zhike Granule after oral administration in rats.
建立了一种灵敏且经过验证的液相色谱-串联质谱法（LC-MS/MS），用于检测芩杏清热止咳颗粒中活性成分的血浆浓度，即栀子苷、甘草苷、异甘草苷、黄芩苷、汉黄芩苷、黄芩素、甘草素、异甘草素和甘草次酸。分析在Ultimate XB-C柱上进行，流速为0.4 mL·min，单次运行时间为18 min。流动相由含0.05%甲酸的水和乙腈组成，采用梯度洗脱。采用正、负离子扫描和选择多反应监测模式进行定量分析。所建立的方法在0.6800 - 340.0至3.920 - 1960 ng·mL的给定范围内具有良好的线性，所有分析物的r > 0.9917。日内和日间精密度（RSD）不超过12%，准确度（RE）小于±11%。提取物回收率和基质效应符合生物样品分析要求。此外，所建立的方法有效地应用于大鼠口服芩杏清热止咳颗粒后的药代动力学研究。
