Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii
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Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii
China PharmacyVol. 32, Issue 16, (2021)
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Published:2021,
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LIU Li, JIANG Hongxia, SUN Qun, et al. Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii. [J]. China Pharmacy 32(16).(2021)
DOI:
LIU Li, JIANG Hongxia, SUN Qun, et al. Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii. [J]. China Pharmacy 32(16).(2021)DOI:
Study on the Mass Spectrometry Fragmentation Regularity and Rapid Identification of Macrocyclic Polyamine Alkaloids from Tripterygium wilfordii
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.