Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education, Harbin 150040, China.
School of Traditional Chinese Medicine, Guangdong Pharmaceutical University, Guangzhou 528458, China.
Molecules. 2019 Feb 8;24(3):598. doi: 10.3390/molecules24030598.
The purpose of this study was to establish a rapid, reliable, and sensitive ultra-performance liquid chromatography with triple-quadrupole tandem mass spectrometry coupled with chemometric method to measure and evaluate the differences between thirteen compounds in raw and processed L. from different sources. This assay method was validated, and the results indicated that the calibration curves for the thirteen compounds had good linearity (R² > 0.9990). The limits of detection and limits of quantification of the thirteen compounds ranged from 0.0012 to 0.0095 μg/mL and from 0.0038 to 0.0316 μg/mL, respectively. The relative standard deviations (RSD) of the intra- and inter-day precisions and stability ranged from 1.06 to 2.00%, 0.26 to 1.99%, and 0.75 to 1.97%, respectively. The sample recovery rates of the thirteen compounds with different concentrations were 94.47⁻104.06%. The chemometric results, including principal component analysis, hierarchical clustering analysis, three-dimensional analysis, and box plot analysis, indicated that there are significance differences in raw and processed L. The results of this study confirm that the proposed method is the first reported method that has been successfully applied for simultaneous determination and discovery of the difference between thirteen compounds of raw and processed L. Thus, this method could be a helpful tool for the detection and confirmation of the quality of traditional Chinese medicines and provide a basis for future pharmacological studies.
本研究旨在建立一种快速、可靠、灵敏的超高效液相色谱三重四极杆串联质谱联用化学计量学方法，用于测定和评价来自不同来源的生地黄和炮制品中 13 种化合物的差异。该方法经过验证，结果表明 13 种化合物的校准曲线具有良好的线性（R²>0.9990）。13 种化合物的检测限和定量限范围分别为 0.0012 至 0.0095 μg/mL 和 0.0038 至 0.0316 μg/mL。日内和日间精密度及稳定性的相对标准偏差（RSD）分别为 1.06%至 2.00%、0.26%至 1.99%和 0.75%至 1.97%。不同浓度的 13 种化合物的样品回收率为 94.47%至 104.06%。化学计量学结果，包括主成分分析、层次聚类分析、三维分析和箱线图分析，表明生地黄和炮制品之间存在显著差异。本研究结果证实，该方法是首次成功应用于同时测定和发现生地黄和炮制品中 13 种化合物差异的方法。因此，该方法可为检测和确认中药质量提供帮助，并为未来的药理研究提供依据。
