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Rapid Isolation of a Dipeptidyl Peptidase IV Inhibitor from Fritillaria cirrhosa by Thin-Layer Chromatography–Bioautography and Mass Spectrometry-Directed Autopurification System
JPC - Journal of Planar Chromatography - Modern TLC ( IF 1.6 ) Pub Date : 2019-12-01 , DOI: 10.1556/1006.2019.32.6.1
Lihua Gu 1, 2 , Tong Tian 1 , Li Xia 1, 2 , Guixin Chou 1, 2 , Zhengtao Wang 1, 2
Affiliation  

A thin-layer chromatography (TLC)-bioautography-mass spectrometry (MS) method coupled with a liquid chromatography- MS-controlled autopurification system was developed and applied for screening and isolating natural dipeptidyl peptidase IV (DPP IV) inhibitor from plant extracts. An unknown constituent with potential DPP IV inhibitory activity from bulbs of Fritillaria cirrhosa was discovered using TLC-bioautography, followed by using a TLC interface with mass spectrometry to obtain m/z of the target compound, and the purification of the compound was directly achieved with a mass-directed autopurification system for 40 runs of injection. Finally, 2.1 mg of the compound was obtained and identified as peimisine by 1H and 13C nuclear magnetic resonance (NMR) spectroscopy. The half maximal inhibitory concentration (IC50) of DPP IV inhibitory activity was determined at 80.5 μm comparing to 58.0 μm of the standard DPP IV inhibitor diprotin A by a spectrophotometric method.

中文翻译:

薄层色谱-生物自传和质谱导向的自动纯化系统从贝母中快速分离二肽基肽酶IV抑制剂

建立了薄层色谱(TLC)-生物自传质谱(MS)结合液相色谱-MS控制的自动纯化系统,并将其用于从植物提取物中筛选和分离天然二肽基肽酶IV(DPP IV)抑制剂。使用TLC-生物自显影技术发现了贝母中具有潜在DPP IV抑制活性的未知成分,然后使用TLC接口和质谱法获得m / z纯化目标化合物,并通过质量导向的自动纯化系统直接进行40次注射纯化。最后,获得2.1mg的化合物,并通过1H和13C核磁共振(NMR)光谱法鉴定为peimisine。通过分光光度法将DPP IV抑制活性的半数最大抑制浓度(IC50)确定为80.5μm,而标准DPP IV抑制剂双protin A为58.0μm。
更新日期:2019-12-01
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