Investigation on Major Constituents in Yangxinshi Tablets Based on HPLC-TOF/MS and HPLC-MS/MS

KeyWord:Yangxinshi tablets  constituents  HPLC-TOF/MS  HPLC-MS/MS  quantitative analysis

Abstract:

      A rapid method for the identification of constituents in Yangxinshi tablets was established by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOF/MS).Simultaneously,the quantitation on the sample was performed by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS).30 kinds of constituents in Yangxinshi tablets were identified by HPLC-TOF/MS in the running conditions as follows:chromatographic column:an Agilent ZORBAX Eclipse Plus C18 column(100 mm¡Á3ª±0 mm,1ª±8 ¦Ìm),mobile phase:acetonitrile-0ª±1% formic acid solution,elution type:gradient elution,flow rate:0ª±2 mL¡¤min-1,column temperature:30 ¡æ,MS scanning mode:electrospray in both positive and negative ion.The HPLC-MS/MS method was operated under the following conditions:chromatographic column:a Waters XBridge¡k BEH C18 column(150 mm¡Á4ª±6 mm,2ª±5 ¦Ìm),mobile phase:acetonitrile-0ª±1% formic acid solution,elution type:gradient elution,flow rate:0ª±4 mL¡¤min-1,column temperature:30 ¡æ,MS scanning mode:multiple reaction monitoring(MRM) mode with electrospray ion source in both positive and negative ion.16 main constituents in Yangxinshi tablets were determined by HPLC-MS/MS.There were excellent linear responses for the peak areas of the analytes to their concentrations with the correlation coefficients(r) not less than 0ª±997.The limits of detection(LODs) and quantitation(LOQs) for 16 constituents were in the range of 0ª±039 1-78ª±1 ¦Ìg/L and 0ª±156-312 ¦Ìg/L,respectively.The average recoveries were in the range of 96ª±8%-103ª±8% with the relative standard deviations of 1ª±0%-3ª±5%.With the advantages of simple operation,accuracy and acceptable reproducibility,the developed method could be applied in the qualitation and quantitation of constituents in Yangxinshi tablets.Therefore,it could provide a reference for the quality control,further study and application of Yangxinshi tablets.