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[利用液相色谱-线性离子阱-轨道阱多级质谱法鉴定浙贝母各部位的生物碱和黄酮类化合物]

[Identification of alkaloids and flavonoids in all parts of Fritillaria thunbergii using LC-LTQ-Orbitrap MSn].

作者信息

Cui Ming-Chao, Zhang Jia-Yu, Chen Shao-Jun, Jiang Hai-Long, Zhou Hai-Bin, Ling Qing-Zhi

机构信息

Zhejiang Pharmaceutical College, Ningbo 315100, China.

Nanjing University of Chinese Medicine, Nanjing 210046, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2016 Jun;41(11):2124-2130. doi: 10.4268/cjcmm20161124.

DOI:10.4268/cjcmm20161124
PMID:28901111
Abstract

Alkaloids and flavonoids in flowers, flower buds, stems, leaves, and bulbs of Fritillaria thunbergii were identified by LC-LTQ-Orbitrap MSn.Alkaloids were identified by ACQUITY UPLC BEH C₁₈(2.1 mm×50 mm, 1.7 μm ) chromatographic column with a mobile phase of 10 mmol•L⁻¹ ammonium formate-acetonitrile and gradient elution in positive MS scan mode.Meanwhile, flavonoids were analyzed by Agilent-Zorbax SB C₁₈ (4.6 mm×250 mm, 5 μm) chromatographic column with a mobile phase of 0.2% acetic acid-acetonitrile and gradient elution in negative MS scan mode.Combined with literature reports, chemical constituents were identified and determined by accurate molecular weights and fragment ion peaks in the ESI-MS/MS spectra based on high resolution mass spectrometer.In all parts of F.thunbergii, 37 alkaloids including 7 alkaloids (zhebeininoside, peimisine, peimine, peiminine, ebeiedinone/puqiedinone, ebeiedine/ puqiedine, peimisine-N-oxide) were simultaneously analyzed.Moreover, 16 flavonoids including quercetin, kaempferol and their glycosides were identified.The results indicated that the aerial parts had the similar alkaloids as the bulbs on the whole.Meanwhile, it had a series of flavonoids undetected in the bulbs.Our results provided the scientific basis for the development and utilization of aerial parts of F.thunbergii.

摘要

采用液相色谱-线性离子阱-轨道阱质谱联用技术(LC-LTQ-Orbitrap MSn)对浙贝母花、花蕾、茎、叶和鳞茎中的生物碱和黄酮类化合物进行了鉴定。生物碱采用ACQUITY UPLC BEH C₁₈(2.1 mm×50 mm,1.7 μm)色谱柱,以10 mmol•L⁻¹甲酸铵-乙腈为流动相,在正离子模式下进行梯度洗脱质谱扫描。同时,黄酮类化合物采用安捷伦-Zorbax SB C₁₈(4.6 mm×250 mm,5 μm)色谱柱,以0.2%乙酸-乙腈为流动相,在负离子模式下进行梯度洗脱质谱扫描。结合文献报道,基于高分辨率质谱仪,通过ESI-MS/MS谱图中的精确分子量和碎片离子峰对化学成分进行了鉴定和测定。在浙贝母的各个部位,同时分析了37种生物碱,其中包括7种生物碱(浙贝宁苷、贝母辛、贝母碱、去氢贝母碱、伊贝啶酮/蒲贝定酮、伊贝啶/蒲贝啶、贝母辛氮氧化物)。此外,还鉴定出了16种黄酮类化合物,包括槲皮素、山柰酚及其糖苷。结果表明,地上部分的生物碱总体上与鳞茎相似。同时,地上部分含有一系列鳞茎中未检测到的黄酮类化合物。我们的研究结果为浙贝母地上部分的开发利用提供了科学依据。

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