Determination of 5 Alkaloids in Fritillaria by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:Fritillaria  alkaloid  ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
  
AuthorInstitution
WANG Wen-wen,YANG Fei,YANG Zhong,FAN Rui,LI Fang,CAO Xue-qin 1.Xinjiang Uyger Autonomous Region Academy of Instrumental Analysis;2.Xinjiang Technical Institute of Physics and Chemistry,Chinese Academy of Sciences
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Abstract:
      A method of ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of five alkaloids,including peimisine,sipeimine,peiminine,peimine and sipeimine 3β-D-glucoside in Fritillaria.Samples were extracted with alkaline methanol-chloroform,and separated on an Acquity UPLC BEH C18 column using acetonitrile solution containing 0.1% formic acid as mobile phase by gradient elution.The target compounds were determined by UPLC-MS/MS under multiple reaction monitoring(MRM) mode,and then quantified by external standard method.The calibration curves showed good linearities in the range of 0.000 5-0.05 mg/L with correlation coefficients(r) greater than 0.999.Recoveries for the five alkaloids at three spiked levels(1.0,2.5,5.0 mg/kg) ranged from 78.6% to 93.1%,with relative standard deviations(RSD) not more than 8.6%.The limits of detection(LOD) and limits of quantitation(LOQ) were 0.03 mg/kg and 0.1 mg/kg,respectively.The established method was simple,sensitive,accurate and reliable,and could be applied in the simultaneous determination of the five alkaloids in Fritillaria.
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