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Study On The Substance Basis Of Xuesaitong Injection Based On UPLC-Orbitrap HRMS

Posted on:2020-03-12Degree:MasterType:Thesis
Country:ChinaCandidate:Y LiuFull Text:PDF
GTID:2504306029493254Subject:Pharmacy
Abstract/Summary:PDF Full Text Request
Objective:UPLC-Orbitrap HRMS was used to separate and identify the content of notoginsenosides in Xuesaitong(lyophilized)for injection and to analyze the chromatographic behavior of the notoginsenoside and the fragmentation of mass spectrometry.Fully utilize the high-energy collision dissociation parameters of mass spectrometry,analyze and assign the secondary fragments and summarize the cleavage rules of the mass spectrometer and the known literature comparison to judge the structural characteristics of the unknown compounds.The establishment of the database for the confirmed comp ounds was performed using the module of the Database Manager in the mass spectrometer Mass Frontier 7.0 software.In order to provide a basis for the material basic research and database establishment of Xuesaitong injection.Methods:Chromatographic conditions: mobile phase: 0.1% formic acid solution(A)-acetonitrile(B);gradient elution,flow rate 1 mL/min;injection volume 10 μL.Mass spectrometry conditions: operating mode: ESI-,Full MS/dd-MS2(Top N)mode,sheath gas flow rate 65 arb,auxiliary gas flow rate 20 arb,purge gas flow rate 4 arb,spray voltage 2.5 kV,capillary(ion transfer tube)The temperature is 300℃,the S-lens voltage is 50 V,and the heating temperature is 500℃.Results:Fifteen saponin compounds were isolated and identified from the blood-plugging(freeze-dried)for injection by column chromatography and analyzed by 13 C NMR and 1H NMR NMR.The final identification results were notoginsenoside R1,Ginsenoside Rg1,Ginsenoside Re,20(S)-Ginsenoside Rf,20(S)-Ginsenoside Rh1,20(S)-Ginsenoside Rg2,Ginsenoside Rb1,20(S)-Ginsenoside F1,Ginsenoside Rb2,Ginsenoside Rc,Ginsenoside Rb3,Ginsenoside Rd,Ginsenoside Rk3,Ginsenoside Rh4,Ginsenoside Rg3.15 saponin compounds were identified by LC-MS and the 15 compounds were identified by Mass Frontier 7.0 software.Conclusion:This study identified 78 saponin compounds and used the Database Manager module in the Mass Frontier 7.0 software from LC-MS to create a database of confirmed compounds.This method has the advantage of rapidly identifying natural compounds and clarifies the material basis of perfusion(freeze-drying)for injection.And to achieve the monitoring of ingredients in order to control the quality of Xuesaitong products.
Keywords/Search Tags:Xuesaitong for injection(lyophilization), LC-MS-DS, Database search
PDF Full Text Request
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