1.上海中医药大学中药研究所,教育部中药标准化重点实验室,中药新资源与品质评价国家中医药管理局重点研究室,上海中药标准化研究中心(上海 201203)
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卢文旭,林李雁,丁玉莲等.基于TLC和TLC⁃EFISI⁃MSn联用技术的霍山石斛专属性鉴别研究[J].上海中医药大学学报,2023,37(05):39-46.
LU Wenxu,LIN Liyan,DING Yulian,et al.Specific identification of Dendrobium huoshanense based on TLC and TLC⁃EFISI⁃MSn combined technology[J].Academic Journal of Shanghai University of Traditional Chinese Medicine,2023,37(05):39-46.
卢文旭,林李雁,丁玉莲等.基于TLC和TLC⁃EFISI⁃MSn联用技术的霍山石斛专属性鉴别研究[J].上海中医药大学学报,2023,37(05):39-46. DOI: 10.16306/j.1008-861x.2023.05.005.
LU Wenxu,LIN Liyan,DING Yulian,et al.Specific identification of Dendrobium huoshanense based on TLC and TLC⁃EFISI⁃MSn combined technology[J].Academic Journal of Shanghai University of Traditional Chinese Medicine,2023,37(05):39-46. DOI: 10.16306/j.1008-861x.2023.05.005.
目的,2,建立霍山石斛薄层色谱(TLC)定性鉴别的质量控制方法,并对霍山石斛专属性成分进行快速结构鉴定。,方法,2,采用TLC法,以水饱和正丁醇为展开剂,低温4 ℃展开,以2%三氯化铝乙醇试液为显色剂,105 ℃加热5 min,于紫外光灯(365 nm)下观察霍山石斛的专属性斑点并进行真伪鉴别;利用原位薄层色谱-静电场诱导喷雾-质谱(TLC-EFISI-MS,n,)联用技术进一步对专属性斑点进行快速结构解析。,结果,2,建立了霍山石斛专属性的TLC鉴别方法,发现霍山石斛有一专属性斑点,通过该斑点可实现霍山石斛与铁皮石斛、紫皮石斛等13种石斛属植物的区分,且能够将霍山石斛粉中掺混20%以上的铁皮石斛粉鉴别出来;根据化合物的相对分子量、多级质谱裂解碎片,初步鉴定该斑点为黄酮类化合物芹菜素-6-,C,-,α,-,L,-鼠李糖基-(1→2)-,β,-D-葡萄糖苷-8-,C,-,α,-,L,-阿拉伯糖,为霍山石斛的专属性成分。,结论,2,所建立的TLC鉴别方法简单灵敏、准确可靠、重现性好且专属性强,为提高霍山石斛的质量控制方法提供了实验依据,对于保证其质量和临床疗效具有重要意义。
Objective: To establish a quality control method for qualitative identification thin-layer chromatograph (TLC) of ,Dendrobium huoshanense, C. Z. Tang et S. J. Cheng by thin-layer chromatography (TLC), and to rapidly identify the specific components of ,D. huoshanense,.,Methods,2,Using water-saturated ,n,-butanol as the developing agent, TLC was developed at a low temperature of 4 ℃. Using a 2% aluminum chloride-ethanol solution as the chromogenic reagent, the developed TLC plate was heated at 105 ℃ for 5 min, then the specific spots of ,D. huoshanense, were observed under ultraviolet light (365 nm) for authenticity identification. ,In situ, thin-layer chromatography-electrostatic field induced spray ionization-mass spectrometry (TLC-EFISI-MS,n,) technology was used for rapid structural analysis.,Results,2,The specific TLC identification method of, D. huoshanense, was established. It was found that there was a specific spot in ,D. huoshanense,, which could be used to distinguish ,D. huoshanense, from 13 species of ,Dendrobium,, such as ,D. officinale ,and, D. devonianum., Furthermore, this method was able to identify more than 20% adulterated ,D. officinale ,powder in ,D. huoshanense, powder. According to the relative molecular weight and multi-stage mass spectrometry fragmentation of the compound, the spot was preliminarily identified as the flavonoid compound apigenin‑6‑,C,‑,α,‑,L,‑rhamnosyl‑(1→2)‑,β,‑,D,‑glucoside‑8‑,C,‑,α,‑,L,‑arabinose, which is the specific component of ,D. huoshanense,.,Conclusion,2,The established TLC identification method is simple, sensitive, accurate and reliable, with good reproducibility and strong specificity. It provides an experimental basis for improving the quality control method of ,D. huoshanense,, and is of great significance for ensuring its quality and clinical efficacy.
霍山石斛薄层色谱薄层色谱-静电场诱导喷雾离子化质谱黄酮苷芹菜素-6-C-α-L-鼠李糖基-(1→2)-β-D-葡萄糖苷-8-C-α-L-阿拉伯糖
D. huoshanensethin-layer chromatography (TLC)thin-layer chromatography-electrostatic field induced spray ionization-mass spectrometry (TLC-EFISI-MSn)flavonol glycosidesapigenin-6-C-α-L-rhamnosyl-(1→2)-β -D-glucoside-8-C-α-L-arabinose
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