Hainan Provincial Key Laboratory of Resources Conservation and Development of Southern Medicine, Hainan Branch of the Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Haikou 570311, China.
School of Life Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, China.
Molecules. 2020 Jan 17;25(2):389. doi: 10.3390/molecules25020389.
, a traditional Chinese medicine, has been used to treat cardio- and cerebrovascular diseases in China for thousands of years. Flavonoids are major active compounds in . In this paper, a rapid and sensitive ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method was developed and validated for simultaneous determination of 17 flavonoids in . Quantification was performed by multiple reaction monitoring using electrospray ionization in negative ion mode. Under the optimum conditions, calibration curves for the 17 analytes displayed good linearity ( > 0.9980). The intra- and inter-day precisions (relative standard deviations) were lower than 5.0%. The limit of quantitation ranged from 0.256 to 18.840 ng/mL. The mean recovery range at three spiked concentrations was 94.18-101.97%. The validated approach was successfully applied to 18 samples of . Large variation was observed for the contents of the 17 analytes. Sativanone and 3'--methylviolanone were the dominant compounds. The fragmentation behaviors of six flavonoids were investigated using UPLC with quadrupole time-of-flight tandem mass spectrometry. In negative ion electrospray ionization mass spectrometry, all the flavonoids yielded prominent [M - H] ions. Fragments for losses of CH, CO, and CO were observed in the mass spectra. Formononetin, liquiritigenin, isoliquiritigenin, sativanone, and alpinetin underwent retro-Diels-Alder fragmentations. The proposed method will be helpful for quality control of .
作为一种传统中药,已在中国被用于治疗心脑血管疾病数千余年。类黄酮是 的主要活性化合物。在本文中,建立并验证了一种快速灵敏的超高效液相色谱-三重四极杆质谱法,用于 中 17 种类黄酮的同时测定。采用电喷雾负离子模式下的多反应监测进行定量分析。在最佳条件下,17 种分析物的校准曲线均具有良好的线性(>0.9980)。日内和日间精密度(相对标准偏差)均低于 5.0%。定量限范围为 0.256-18.840ng/mL。在三个加标浓度下,平均回收率范围为 94.18-101.97%。该方法已成功应用于 18 个 样品的分析。在 17 种类黄酮的含量方面观察到了很大的差异。萨替宁酮和 3'--甲基香草酮为主要化合物。采用超高效液相色谱-四极杆飞行时间串联质谱法研究了六种类黄酮的裂解行为。在负离子电喷雾电离质谱中,所有类黄酮均产生明显的[M-H]离子。在质谱中观察到 CH、CO 和 CO 的丢失碎片。芒柄花素、甘草素、异甘草素、萨替宁酮和川陈皮素发生逆狄尔斯-阿尔德裂解。所提出的方法将有助于 的质量控制。