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目的:建立高效液相色谱-电喷雾-质谱(HPLC-ESI-MS)方法,分析比较山茱萸炮制前后化学成分的变化。方法:采用Agilent Extend-C18色谱柱,乙腈-0.1%甲酸水溶液梯度洗脱;Agilent1200高效液相色谱仪—6410三重四级杆质谱仪联用;正、负离子检测模式。结果:通过质谱中的主要碎片,在正离子检测模式下,山茱萸生品中检测出了莫诺苷、马钱苷、山茱萸裂苷,制品中检测出了5-羟甲基糠醛、莫诺苷、马钱苷和山茱萸裂苷;在负离子检测模式下,山茱萸生、制品中均检测出了没食子酸、7-O-没食子酰基景天庚酮糖、莫诺苷、山茱萸裂苷。结论:在质谱正、负离子检出模式下,主要化学成分响应均较好,这为分析山茱萸炮制前后化学成分变化,以及控制饮片质量提供了一种新的方法。
Objective: To establish a high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method to analyze and compare the chemical composition before and after processing Cornus officinalis. Methods: An Agilent Extend-C18 column was used with gradient elution of acetonitrile-0.1% formic acid. The Agilent 1200 high performance liquid chromatography-6410 triple quadrupole mass spectrometer was used together with positive and negative ion detection mode. Results: Morroniside, loganin and arctoside were detected in the samples of Fructus Corni in the positive ion detection mode by the main fragments in the mass spectrometry. 5-Hydroxymethylfurfural and morroniside , Loganin and argillaceae glycosides. In the negative ion detection mode, the contents of gallic acid, 7-O-gallic acid scopolamine, morroniside and dogwood glycosides were all detected in the raw materials of dogwood. Conclusion: In the positive and negative ion mass spectrometry modes, the main chemical components respond well, which provides a new method for analyzing the chemical composition changes before and after processing Cornus officinalis and controlling the quality of the slices.