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采用 UHPLC-QQQ-MS/MS 同时测定多种生物碱,发现改善青风藤茎质量和安全性控制的化学标志物。

Discovery of chemical markers for improving the quality and safety control of Sinomenium acutum stem by the simultaneous determination of multiple alkaloids using UHPLC-QQQ-MS/MS.

机构信息

Faculty of Chinese Medicine and State Key Laboratory of Quality Research in Chinese Medicine, Macau University of Science and Technology, Taipa, Macao, People's Republic of China.

Institute of International Standardization of Traditional Chinese Medicine, Shanghai University of Traditional Chinese Medicine, Shanghai, 201203, People's Republic of China.

出版信息

Sci Rep. 2020 Aug 25;10(1):14182. doi: 10.1038/s41598-020-71133-4.

Abstract

Sinomenium acutum stem is a popular traditional Chinese medicine used to treat bone and joint diseases. Sinomenine is considered the only chemical marker for the quality control of S. acutum stem in mainstream pharmacopeias. However, higenamine in S. acutum stem is a novel stimulant that was banned by the World Anti-Doping Agency in 2017. Therefore, enhancing the quality and safety control of S. acutum stem to avoid potential safety risks is of utmost importance. In this study, a fast, sensitive, precise, and accurate method for the simultaneous determination of 11 alkaloids in S. acutum stem by ultrahigh-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UHPLC-QQQ-MS/MS) was established. This method successfully analyzed thirty-five batches of S. acutum stem samples. The average contents of sinomenine, magnoflorine, coclaurine, acutumine, higenamine, sinoacutine, palmatine, magnocurarine, columbamine, 8-oxypalmatine, and jatrorrhizine were 24.9 mg/g, 6.35 mg/g, 435 μg/g, 435 μg/g, 288 μg/g, 44.4 μg/g, 22.5 μg/g, 21.1 μg/g, 15.8 μg/g, 9.30 μg/g, and 8.75 μg/g, respectively. Multivariate analysis, including principal component analysis (PCA), orthogonal partial least square method-discriminant analysis (OPLS-DA), and hierarchical cluster analysis (HCA), were performed to characterize the importance and differences among these alkaloids in S. acutum stem samples. As a result, sinomenine, magnoflorine, coclaurine, acutumine, and higenamine are proposed as chemical markers for quality control. Higenamine and coclaurine are also recommended as chemical markers for safety control. This report provides five alkaloids that can be used as chemical markers for improving the quality and safety control of S. acutum stem. It also alerts athletes to avoid the risks associated with consuming S. acutum stem.

摘要

青风藤是一种常用的传统中药,用于治疗骨骼和关节疾病。在主流药典中,青藤碱被认为是青风藤质量控制的唯一化学标志物。然而,青风藤中的盐酸育亨宾是一种新型兴奋剂,已于 2017 年被世界反兴奋剂机构禁用。因此,提高青风藤的质量和安全性控制,以避免潜在的安全风险至关重要。本研究建立了一种超高效液相色谱-三重四极杆串联质谱(UHPLC-QQQ-MS/MS)同时测定青风藤中 11 种生物碱的快速、灵敏、准确、精确的方法。该方法成功分析了 35 批青风藤样品。青藤碱、粉防己碱、蝙蝠葛碱、青藤碱、盐酸育亨宾、青风藤碱、延胡索乙素、木兰碱、小檗碱、氧化黄连碱和吴茱萸碱的平均含量分别为 24.9μg/g、6.35μg/g、435μg/g、435μg/g、288μg/g、44.4μg/g、22.5μg/g、21.1μg/g、15.8μg/g、9.30μg/g和 8.75μg/g。采用主成分分析(PCA)、正交偏最小二乘法判别分析(OPLS-DA)和层次聚类分析(HCA)等多元分析方法对青风藤样品中这些生物碱的重要性和差异进行了表征。结果表明,青藤碱、粉防己碱、蝙蝠葛碱、青藤碱和盐酸育亨宾可作为质量控制的化学标志物。盐酸育亨宾和蝙蝠葛碱也被推荐为安全性控制的化学标志物。本报告提供了 5 种可用于提高青风藤质量和安全性控制的化学标志物。同时也提醒运动员避免摄入青风藤带来的风险。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/30f9/7447749/b5b943b1184d/41598_2020_71133_Fig1_HTML.jpg

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