雷公藤大环多胺类生物碱的质谱裂解规律及其快速识别研究
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篇名: 雷公藤大环多胺类生物碱的质谱裂解规律及其快速识别研究
TITLE: Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii
摘要: 目的:研究雷公藤大环多胺类生物碱的质谱裂解规律,建立快速识别该类生物碱的方法。方法:在色谱柱为HypersilGOLDTMC18、流动相为0.1%甲酸溶液(A)-甲醇(B)(梯度洗脱)、流速为0.25mL/min、柱温为40℃、进样量为2μL的色谱条件下,以及在离子源为电喷雾离子源、扫描模式为正离子模式、裂解电压为100V、碰撞能量为35eV、扫描范围为m/z100~2000的质谱条件下,采用超高效液相色谱-四极杆-飞行时间串联质谱技术(UPLC-Q-TOF-MS/MS)结合PeakView1.2软件分析celafurine、celabenzine、celacarfurine和celacinnine等4个大环多胺生物碱对照品和雷公藤总提取物的质谱信息,并总结该类生物碱的质谱裂解规律。根据保留时间、精确分子量及二级质谱碎片离子信息,参照上述质谱裂解规律,对雷公藤总提取物中大环多胺生物碱成分进行快速识别,并通过查阅Scifinder数据库及文献比对判断其是否为新化合物。结果:在正离子扫描模式下,m/z160.11(基峰)、m/z188.10和m/z100.07为大环多胺生物碱的二级质谱特征裂解碎片离子。根据精确分子量和质谱裂解规律从雷公藤总提取物中快速识别大环多胺生物碱10个,其中化合物1~6、8分别为2-phenyl-1,5,9-triazacyclotridecan-4-one、9-acetyl-2-phenyl-1,5,9-triazacyclotridecan-4-one、9-nicotinoyl-2-phenyl-1,5,9-triazacyclotridecan-4-one、celafurine、celabenzine、celacarfurine、celacinnine,其余3个化合物结构待定。化合物3、7、9和10可能为新的化合物。结论:大环多胺生物碱能够形成m/z160.11(基峰)、m/z188.10和m/z100.07等3个共同特征碎片离子,可用于该类活性成分的快速识别。
ABSTRACT: OBJECTIVE:To stud y the mass spec trometry fragmentation regularity and establish rapid identification method of macrocyclic polyamine alkaloids from Tripterygium wilfordii. METHODS :The determination was performed on Hypersil GOLDTM C18 column with 0.1% formic acid solution (A)-methanol(B)as mobile phase (gradient elution )at the flow rate of 0.25 mL/min. The column temperature was 40 ℃,and sample size was 2 μL. The mass spectrometric condition included ESI,positive ion mode , breakdown voltage of 100 V,collision energy of 35 eV,and scanning range of m/z 100-2 000. UPLC-Q-TOF-MS/MS combined with PeakView 1.2 software were used to analyze mass spectrum of 4 macrocyclic polyamine alkaloids control as celafurine , celabenzine,celacarfurin,celacinnine and total extract of T. wilfordii ,and summarized the mass fragmentation regularity of alkaloids. According to retention time ,accurate molecular weight and secondary mass fragment ion information ,referring to the above mass spectrometry fragmentation regularity ,macrocyclic polyamine alkaloids in the total extract of T. wilfordii were quickly identified,and whether it was a new compound was determined by consulting Scifinder database and literature comparison. RESULTS:There were three characteristic cleavage fragments of macrocyclic polyamine alkaloids ,i.e. m/z 160.11(base peak ),m/z 188.10 and m/z 100.07 in positive ion mode. According to the precise molecular weight and mass spectrometry fragmentation regularity,10 macrocyclic polyamine alkaloids were identified rapidly ,and compound 1-6,8 were 2-phenyl-1,5,9-triazacy- clotridecan-4-one, 9-acetyl-2-phenyl-1,5,9-triazacyclotridecan-4-one, 9-nicotinoyl-2-phenyl-1, 5, 9-triazacyclotridecan-4-one, celafurine,celabenzine,celacarfurine,celacinnine,respectively. Compounds 3,7,9 and 10 might be new compounds. CONCLUSIONS:The macrocyclic polyamine alkaloids canform three common characteristic fragment ions ,m/z 160.11(base peak ),m/z 188.10 and m/z 100.07,which can be used for the rapid identification of these active components.
期刊: 2021年第32卷第16期
作者: 刘莉,蒋红霞,孙群,陈殊,刘建群
AUTHORS: LIU Li,JIANG Hongxia ,SUN Qun,CHEN Shu,LIU Jianqun
关键字: 雷公藤;大环多胺生物碱;质谱裂解规律;快速识别
KEYWORDS: Tripterygium wilfordii; Macrocyclic polya-
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