Determination of Six Alkaloids in Ervatamia Officinalis Tsiang by Ultra High Performance Liquid Chromatography£­Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

KeyWord:Ervatamia officinalis Tsiang  alkaloid  dispersive solid phase extraction  ultra high performance liquid chromatography£­tandem mass spectrometry

Abstract:

      An ultra high performance liquid chromatography£­tandem mass spectrometry£¨UPLC£­MS/MS£© with dispersive solid phase extraction£¨dSPE£© was developed for the simultaneous determination of six alkaloids in Ervatamia officinalis Tsiang£®Effects of the dSPE experimental conditions on the extraction efficiency for six alkaloids were investigated by single factor£®The optimum conditions showed that the ratio of solid to liquid£¨g¡ÃmL£© was 1¡Ã20 with 1% ammonia methanol as solvent£¬and the amount of PSA and NH2 mixed adsorbent was 200 mg£®After dSPE extraction£¬the sample was analyzed by UPLC£­MS/MS with acetonitrile and 0.1% ammonium formate as mobile phases£®Results showed that there were good linear relationships for six alkaloids in the range of 1£­100 mg/L£¬with their correlation coefficients not lower than 0.983 7£®The limits of detection and limits of quantitation were in the range of 0.05£­0.10 mg/L and 0.15£­0.35 mg/L£¬respectively£®The recoveries at three spiked levels of 1£¬10 and 50 mg/L ranged from 93.2% to 98.1%£¬with relative standard deviations£¨RSDs£© not more than 2.9%£®The method was used for the determination of six alkaloids in the samples from 6 habitats£¬with their contents of 0.07£­0.86 mg/g£®The spiked recoveries were in the range of 91.5%£­98.6%£¬with RSDs of 1.1%£­2.9%£®The method is accurate£¬sensitive£¬rapid and simple£¬and it could meet the requirements for detection of the alkaloids in Ervatamia officinalis Tsiang.