采用 UHPLC-Q-Exactive MS、TLC 自显影法和 DART-MS 对滇黄芩进行定性和定量分析。
Qualitative and quantitative analysis of Porana sinensis Hemsl by UHPLC-Q-Exactive MS, TLC autographic method and DART-MS.
机构信息
The MOE Key Laboratory for Standardisation of Chinese Medicines and the Shanghai Key Laboratory for Compound Chinese Medicines, Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai, China.
Shaanxi Academy of Traditional Chinese Medicine, Xi'an, China.
出版信息
Phytochem Anal. 2019 May;30(3):311-319. doi: 10.1002/pca.2814. Epub 2018 Dec 19.
INTRODUCTION
Erycibe obtusifolia and E. schmidtii are widely used in traditional Chinese medicine (TCM) to treat joint pain and rheumatoid arthritis. With the reduction of wild E. obtusifolia and E. schmidtii resources, Porana sinensis has been widely used as a substitute. However, few studies have been conducted on the chemical composition and quality control of P. sinensis.
OBJECTIVE
To clarify the chemical composition and improve the quality control of P. sinensis.
METHODOLOGY
We developed an ultra-high performance liquid chromatography electrospray ionisation Q-Exactive Focus tandem mass spectrometry (UHPLC-ESI-Q-Exactive Focus-MS/MS) method to characterise the chemical constituents of P. sinensis. A strategy based on a combination of high-performance thin-layer chromatography (HPTLC) and direct analysis in real-time (DART) ion source was proposed for the identification of alkaloid components in P. sinensis. Thin-layer chromatography (TLC) autography for 2,2'-diphenyl-1-picrylhydrazyl free radical (DPPH˙) and TLC bioautography for xanthine oxidase were used to rapidly screen marker compounds for high-performance liquid chromatography (HPLC) determination of P. sinensis. Based on the selected marker compounds, a HPLC method for the quantitative determination of eight marker compounds in P. sinensis was developed.
RESULTS
Eighteen compounds in P. sinensis were identified by UHPLC-Q-Exactive MS. Taken together with the results of TLC autography and TLC bioautography, eight compounds were chosen as marker compounds for HPLC determination of P. sinensis. The alkaloid components in P. sinensis were identified as Baogongteng A and Baogongteng C by DART-MS.
CONCLUSION
We systematically clarified the chemical composition of P. sinensis for the first time, and potentially improved its quality control. These results should promote the application of P. sinensis as a new resource for Caulis Erycibes.
简介
水麻叶和滇水麻在传统中药中被广泛用于治疗关节痛和类风湿关节炎。随着野生水麻叶和滇水麻资源的减少，豆腐柴已被广泛用作替代品。然而，目前针对豆腐柴的化学成分和质量控制研究较少。
目的
阐明豆腐柴的化学成分并提高其质量控制。
方法
我们开发了一种超高效液相色谱-电喷雾离子源- Q-Exactive Focus 串联质谱（UHPLC-ESI-Q-Exactive Focus-MS/MS）方法来表征豆腐柴的化学成分。提出了一种基于高效薄层色谱（HPTLC）和实时直接分析（DART）离子源相结合的策略，用于鉴定豆腐柴中的生物碱成分。采用 2,2'-二苯基-1-苦基肼自由基（DPPH˙）薄层色谱自显影和黄嘌呤氧化酶薄层色谱生物自显影，快速筛选用于豆腐柴高效液相色谱（HPLC）测定的标记化合物。基于所选的标记化合物，建立了一种用于定量测定豆腐柴中 8 种标记化合物的 HPLC 方法。
结果
通过 UHPLC-Q-Exactive MS 鉴定了豆腐柴中的 18 种化合物。结合薄层色谱自显影和薄层色谱生物自显影的结果，选择 8 种化合物作为 HPLC 测定豆腐柴的标记化合物。通过 DART-MS 鉴定了豆腐柴中的生物碱成分为包公藤甲和包公藤丙。
结论
我们首次系统地阐明了豆腐柴的化学成分，可能提高了其质量控制。这些结果应促进将豆腐柴作为一种新的蛇菰科资源的应用。
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