ABSTRACT
A high performance liquid chromatography with a diode array detector combined with electrospray ionization ion trap time-of-flight multistage mass spectrometry(HPLC-DAD-ESI-IT-TOF-MS~n, HPLC-MS~n) method was established for qualitative analysis of the chemical components of ethyl acetate extract from Sinopodophylli Fructus. The analysis was performed on a Kromasil 100-5 C_(18)(4.6 mm×250 mm, 5 μm) column, with a mobile phase consisted of 0.1% formic acid(A) and acetonitrile(B) for gradient at a flow rate of 1.0 mL·min~(-1). Electrospray ionization ion trap time-of-flight multistage mass spectrometry was applied for qualitative analysis under positive and negative ion modes. With use of reference substance, characteristic fragmentation and their HR-MS data, 102 components were identified, including 67 flavonoids and 35 lignans. Among them, 45 compounds were reported in Sinopodophylli Fructus for the first time and 19 compounds were identified as new compounds. PharmMapper was used to predict the bioactivity of compounds that were first reported in Sinopodophylli Fructus, and 20 compounds of them were identified to have potential anticancer activity. The results showed that there were many isomers in the ethyl acetate extract of Folium Nelumbinis, and a total of 19 groups of isomers were found. Among them, C_(21)H_(20)O_8 had the highest number of isomers(18 compounds), all of which were α-peltatin or its isomers; C_(21)H_(20)O_7 ranked second, with 10 compounds, all of which were 8-prenylquercetin-3-methyl ether or its isomers. In conclusion, an HPLC-MS~n method was established for qualitative analysis of the ethyl acetate extract(with anti-breast cancer activity) from Sinopodophylli Fructus in this study, which will provide the evidence for clarifying pharmacological active ingredients of the ethyl acetate extract from Sinopodophylli Fructus against breast cancer.
Subject(s)
Acetates , Chromatography, High Pressure Liquid , Fruit , Spectrometry, Mass, Electrospray IonizationABSTRACT
Objective To investigate the ex tr action technique for seperating the active components in the root of Salvia mi ltiorrhizae bunge by supercritical fluid, and to analyze the extracted product s by HPLC-MS n . Methods The extraction condition s were established as follows: 950ml?L -1ethanol as the first entrainer, t he pressure of 20.0 MPa, temperature at 45 ℃, and extracting time 1 h; then 100 mL?L -1 ethanol was selected as the second entrainer, pressur e was 30.0 MPa, temperature was 65 ℃, and extracting time was 3 h. Results Compared with traditional refluxing extraction and ultrasonic extraction, supercritical fluid extraction was better and more effect ive. Conclusion Supercritical extraction is simple, highly selec tive and efficient in extracting the active components in Salvia miltiorrhizae bunge.
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AIM: To establish methods for identifying the antetype of Compound Qingkailing(Calculus bovis,Concha margaritifera,Radix isatidis,Cornu bubali) in rat serum by HPLC-MS~n and HPLC-TOF-MS. METHODS: Addition of methanol to serum after Qingkailing given intravenously to rats was used to precipitate protein.The HPLC-TOF-MS provided the exact molecular weight and the HPLC-ESI-MS~n provided the m/z of multilevel fragment.The medicine antetypes were identified by combining the two methods. RESULTS: Four main medicine antetypes in rat serum,such as geniposide,baicalein,wogonoside and cholic acid,were identified. CONCLUSION: It is a rapid and exact method that can be used to identify other complicated traditional Chinese medicine in vivo.
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AIM: To study the chemical components in Compound Kushen Injection(Radix Sophorae Flavescentis),and to develop a method to identify the composition contained Radix Sophorae Flavescentis. METHODS: The sample was analysed with gradient elution by HPLC.Agilent MS TRAP equipped with ESI source was used as detector and operated in positive ion mode. RESULTS: 11 components were identified in Compound Kushen Injection. CONCLUSION: This method is simple,rapid and can be used for the analysis of components in Compound Kusen Injection.