Institute for Innovative Drug Design and Evaluation, School of Pharmacy, Henan University, N. Jinming Ave., Kaifeng, Henan 475004, China; Institute of Chinese Material Medica, China Academy of Chinese Medical Sciences, Beijing 100102, China.
Institute of Chinese Material Medica, China Academy of Chinese Medical Sciences, Beijing 100102, China.
J Pharm Biomed Anal. 2019 Jan 30;163:105-112. doi: 10.1016/j.jpba.2018.08.058. Epub 2018 Aug 28.
A new ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometry was developed to evaluate the quality of Tanreqing injection. Seven flavonoids (Rutin, Baicalin, Scutellarin, Chrysin-7-O-Beta-d-glucoronide, Oroxylin A-7-O-β-d-glucoronide, Wogonin, Luteolin-7-O-glucoside), two phenolic acids (Chlorogenic acid, Caffeic acid) and two cholesterines (Ursodeoxycholic acid, Chenodeoxycholic acid) in Tanreqing injection could be measured simultaneously. For the determination of the eleven compounds, the conditions were set as follows: The mobile phase was a gradient of 0.1% aqueous formic acid solution (A) and acetonitrile (B); the flow rate was 0.2 mL min, the column was Acquity UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm); and the multiple-reaction monitoring (MRM) with a negative electro spray ionization interface (ESI-) was selected. Within the test ranges, all the standard regression curves showed excellent linear regression (r > 0.99). In terms of (relative standard deviation) RSDs, the precision, repeatability and stability of the eleven compounds were all lower than 3%. The recovery rates of Tanreqing injection and the RSD were 97.8-103.7% and 0.4%-2.0%, respectively. The RSD value was in accordance with the requirements of less than 3.0%. This method has been successfully used in the analysis of Tanreqing injection. In summary, a fast, accurate and reliable UPLC-ESI-MS/MS method was successfully developed for the simultaneous detection of the eleven major active ingredients with different chemical structures in Tanreqing injection, and can be used for the quality control of Tanreqing injection as well.
建立了一种新的超高效液相色谱-三重四极杆质谱联用方法，用于评价痰热清注射液的质量。该方法可以同时测定痰热清注射液中的 7 种黄酮类成分（芦丁、黄芩苷、汉黄芩素、白杨素-7-O-β-D-葡萄糖醛酸苷、黄芩素-7-O-β-D-葡萄糖醛酸苷、木樨草素、芹菜素-7-O-葡萄糖苷）、2 种酚酸类成分（绿原酸、咖啡酸）和 2 种胆甾醇类成分（熊去氧胆酸、鹅去氧胆酸）。在测定这 11 种化合物时，采用的条件如下：流动相为 0.1%甲酸水溶液（A）-乙腈（B）梯度洗脱，流速为 0.2ml/min，色谱柱为 Acquity UPLC HSS T3 柱（2.1mm×100mm，1.8μm），采用负离子电喷雾电离（ESI-）接口的多反应监测（MRM）模式。在测试范围内，所有标准回归曲线均显示出良好的线性关系（r＞0.99）。就（相对标准偏差）RSD 而言，这 11 种化合物的精密度、重复性和稳定性均低于 3%。痰热清注射液的回收率和 RSD 分别为 97.8%-103.7%和 0.4%-2.0%，RSD 值符合不超过 3.0%的要求。该方法已成功应用于痰热清注射液的分析。综上所述，本研究建立了一种快速、准确、可靠的 UPLC-ESI-MS/MS 法，可同时检测痰热清注射液中 11 种具有不同化学结构的主要活性成分，可用于痰热清注射液的质量控制。
