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目的:对桑白皮总黄酮提取物中的各化合物进行快速的分离和鉴定,并对其主要的裂解碎片和二级裂解规律进行探讨。方法:采用超高效液相串联四级杆飞行时间质谱联用技术(UPLC-Q-TOF-MS),在电喷雾离子源(ESI)负离子模式下进行分离和检测;使用Waters公司BRH分析柱(2.1 mm×50 mm,1.7μm);以0.1%甲酸水为流动相A,乙腈为流动相B,梯度洗脱;流速0.3 m L·min~(-1);柱温为25℃。结果:基于UPLC-Q-TOF-MS技术分离所得精确相对分子质量,结合二级质谱裂解信息,使用Masslynx 4.1软件对数据进行统计和分析,并参考Sci Finder数据库(美国化学学会在线数据库学术版),桑白皮总黄酮提取物中共鉴定出13种黄酮成分,其中有7个Diels-Alder加合物,主要代表物为桑根酮C(sanggenon C),桑根酮D(sanggenon D),6种异戊烯基黄酮类化合物,代表物为桑辛素(morusin)。结论:通过超高效液相的分离,首次发现了桑白皮总黄酮提取物中的化合物在ESI源中脱去H_2和H_2O的现象,并对其二级裂解碎片的规律进行探讨,同时也为桑白皮总黄酮提取物的成分鉴定提供了一个快速、简便、可靠的方法。
OBJECTIVE: To rapidly isolate and identify the compounds from the total flavonoids extracts of Morus alba, and discuss the main cracking fragments and secondary cracking rules. METHODS: The separation and detection were carried out in ESI negative ion mode by using UPLC-Q-TOF-MS with ultra-high performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry. 2.1 mm × 50 mm, 1.7 μm). The mobile phase consisted of 0.1% formic acid as mobile phase A and acetonitrile as mobile phase B with a gradient of 0.3 m L · min -1. The column temperature was 25 ℃. Results: Based on the UPLC-Q-TOF-MS technique, the accurate relative molecular mass was separated, and the information of secondary mass spectrometry cleavage was combined with the data of Masslynx 4.1 software for statistics and analysis. The Sci Finder database (American Chemical Society Online Database Academic Version) Thirteen flavonoids were identified from the total flavonoids extracts of Morus alba, including seven Diels-Alder adducts, the main representatives were sanggenon C, sanggenon D, Species isopentenyl flavonoids, the representative for the morinin (morusin). CONCLUSION: The separation of H 2 O 2 and H 2 O from the total flavonoids extract of Morus alba in the ESI source was first found by the separation of ultra-high performance liquid phase, and the rules of the secondary cracking fragments were also discussed Morus alba white flavonoids extract composition identification provides a quick, easy and reliable method.