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采用 UPLC-QTOF-MS/MS 化学特征图谱结合 UPLC-TQ-MS/MS 定量分析方法整体评价槐米质量。

Holistic quality evaluation of Hibisci Mutabilis Folium by integrating UPLC-QTOF-MS/MS chemical profiling and UPLC-TQ-MS/MS quantification approaches.

机构信息

Department of Pharmaceutical Analysis, Affiliated hospital of Integrated Traditional Chinese and Western Medicine, Nanjing University of Chinese Medicine, Nanjing 210028, China; Department of Metabolomics, Jiangsu Province Academy of Traditional Chinese Medicine and Jiangsu Branch of China Academy of Chinese Medical Sciences, Nanjing 210028, China.

Department of Pharmaceutical Analysis, Affiliated hospital of Integrated Traditional Chinese and Western Medicine, Nanjing University of Chinese Medicine, Nanjing 210028, China.

出版信息

J Pharm Biomed Anal. 2022 Sep 5;218:114869. doi: 10.1016/j.jpba.2022.114869. Epub 2022 Jun 3.

Abstract

In present study, an integrating UPLC-QTOF-MS/MS chemical profiling and UPLC-TQ-MS/MS quantification strategy was developed for the holistic quality evaluation of Hibisci Mutabilis Folium (HMF), a traditional Chinese medicinal herb. Using UPLC-QTOF-MS/MS, a total of 58 components were characterized in HMF sample, of which 36 flavonoids, 3 coumarins, 7 organic acids and 4 triterpene acids were unambiguously identified by comparing the chromatographic behavior and mass spectrum with that of reference compounds, or tentatively assigned by comparing the fragmentation pathways and characteristic fragment ions with that of reference substances and/or published literatures together with mass defect filtering (MDF) screening. Meanwhile, 29 representative major components, including 16 flavonoids, 3 coumarins, 7 organic acids and 3 triterpene acids, were quantified by a newly established UPLC-TQ-MS/MS method that was validated in terms of linearity, sensitivity, precision, repeatability, accuracy and stability. The integrated strategy was applied to simultaneously qualifying and quantifying HMF commercial samples and self-prepared samples harvested in difference periods and dried with different methods. It was found that the contents of 29 major components were obviously different in commercial samples or self-prepared samples, suggesting that the holistic quality of HMF commercial samples was inconsistent, and harvesting period and drying method might be the main factors that affect the holistic quality consistency of commercial HMF samples. Standardized harvesting period and drying method should be established for ensuring the holistic quality consistency of HMF.

摘要

在本研究中,开发了一种整合 UPLC-QTOF-MS/MS 化学分析和 UPLC-TQ-MS/MS 定量策略,用于整体质量评估传统中药木槿叶(HMF)。使用 UPLC-QTOF-MS/MS,共鉴定出 HMF 样品中的 58 种成分,其中 36 种黄酮类化合物、3 种香豆素类化合物、7 种有机酸和 4 种三萜酸通过比较色谱行为和质谱与对照化合物进行了明确的鉴定,或通过比较碎片途径和特征碎片离子与对照物质和/或已发表文献并结合质量缺陷过滤(MDF)筛选进行了初步鉴定。同时,通过建立的 UPLC-TQ-MS/MS 方法对 29 种代表性主要成分(包括 16 种黄酮类化合物、3 种香豆素类化合物、7 种有机酸和 3 种三萜酸)进行了定量分析,并对该方法进行了线性度、灵敏度、精密度、重复性、准确性和稳定性验证。该综合策略用于同时定性和定量分析 HMF 商业样品和不同时期收获并采用不同方法干燥的自制样品。结果发现,商业样品或自制样品中的 29 种主要成分的含量明显不同,表明商业 HMF 样品的整体质量不一致,收获期和干燥方法可能是影响商业 HMF 样品整体质量一致性的主要因素。为保证 HMF 的整体质量一致性,应制定标准化的收获期和干燥方法。

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