Identification and quantification of the anti-inflammatory constituents in Pian-Tze-Huang by liquid chromatography combined with quadrupole time-of-flight and triple quadrupole mass spectrometry
Identification and quantification of the anti-inflammatory constituents in Pian-Tze-Huang by liquid chromatography combined with quadrupole time-of-flight and triple quadrupole mass spectrometry
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液相色谱结合四极杆飞行时间和三重四极杆质谱法鉴定和定量片子黄中的抗炎成分
DOI：
10.1016/j.jchromb.2016.05.021
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发表时间：
2016-08-01
影响因子：
3
通讯作者：
Lu, Jinjian
中科院分区：
文献类型：
--
作者：
Huang, Mingqing;Xu, Wen;Lu, Jinjian
采用定性定量分析结合活性评价的方法，对我国已有460年历史的珍贵含片片仔癀（PZH）进行了综合质量控制研究。在定性分析中，开发了一种高性能 LC-四极杆飞行时间 MS 方法来鉴定 PZH 中的化学成分。通过与对照品比较，明确鉴定出27个化合物，并根据MS数据并与文献比较，初步推导出12个化合物。然后对27个化合物的体外抗炎活性进行了评价，其中9个皂苷、11个胆汁酸、牛磺酸和麝香酮对TNF-α产生具有显着的抑制活性，IC50值范围为12.34至147.24μM。在定量分析中，采用超高效LC-三重四极杆质谱仪同时检测15批PZH样品中的21个活性化合物作为质量控制标志物。所有分析物均在 15 分钟内检测到。线性范围宽，判定系数精细（r(2) > 0.9990），具有令人满意的线性度。日内和日间精密度、重复性、稳定性和回收率的相对标准偏差分别小于4.32%、4.94%、4.78%、4.87%和4.91%。本研究建立了一种高灵敏、高效的PZH综合质量控制方法，包括定性定量分析与药理活性评价相结合。 (C) 2016 Elsevier B.V. 保留所有权利。
Both qualitative and quantitative analyses combined with activity evaluation were used for the integrated quality control study of Pien-Tze-Huang (PZH), a precious lozenge used for 460 years in China. In qualitative analysis, a high performance LC-quadrupole time-of-flight MS method was developed for the identification of chemical profiling in PZH. 27 compounds were unambiguously identified by comparing with reference substances, and 12 compounds were tentatively deduced based on their MS data and comparing with literatures. Then the in vitro anti-inflammatory activity of 27 compounds were evaluated, and 9 saponins, 11 bile acids, taurine and muscone exhibited significant inhibitory activities on TNF-alpha production with IC50 values ranging from 12.34 to 147.24 mu M. In quantitative analysis, 21 active compounds, selected as quality control markers, were simultaneously detected in 15 batches of PZH samples by ultra-performance LC-triple quadrupole MS. All the analytes were detected within 15 min. Satisfactory linearity was achieved with wide linear range and fine determination coefficient (r(2) > 0.9990). The respective relative standard deviations of intra- and inter-day precisions, repeatability, stability, and recovery were less than 4.32%, 4.94%, 4.78%, 4.87%, and 4.91%. This study established a high sensitive and efficient method for the integrated quality control of PZH, including qualitative and quantitative analyses combined with pharmacological activity evaluation. (C) 2016 Elsevier B.V. All rights reserved.