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| Simultaneous Determination of 5 Main Flavone Aglycones in Lonicerae Flos by Solid Phase Extraction Purification and Liquid Chromatography Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:Lonicerae Flos flavone aglycones solid phase extraction liquid chromatography tandem mass spectrometry(LC-MS/MS) |
| Author | Institution |
| SHI Ying-zhu,HOU Jian-bo,XIE Wen,YAO Bin-bin,SHENG Tao,HU Xiao-li,ZHANG Hui |
1.The College of Biosystems Engineering and Food Science of Zhejiang University,Hangzhou,China;2.The Technic Center of Hangzhou Customs,Hangzhou,China;3.Zhejiang Academy of Science and Technology for Inspection and Quarantine,Hangzhou,China;4.Zhejiang Lead Product Technic Co.Ltd.,Hangzhou,China |
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| Abstract: |
| In this paper,an analytical method were developed for the determination of 5 main flavone aglycones including quercetin,luteolin,kaempferol,apigenin and baicalein,in Lonicerae Flos by solid phase extraction and liquid chromatography tandem mass spectrometry(SPE/LC-MS/MS).In Lonicerae Flos samples,rutin,cynaroside,astragalin,rhoifolin and baicalin were hydrolyzed and extracted by 50% ethanol solution(contained 10% hydrochloric acid),refluxed for 120 min,and finally cleaned up with an HLB solid phase extraction column.The solution was separated on a Mightysil RP-18 column(150 mm×46 mm(id),3 μm),and determined by LC-MS/MS with negative electrospray ionization(ESI-) in multiple reaction monitoring(MRM) mode.The external standard method was used for the quantitation analysis of 5 main flavone aglycones.The limits of quantitation(LOQs,S/N=10) were 0005 g/kg for quercetin,001 g/kg for luteolin and apigenin,and 005 g/kg for kaempferol and baicalein.Single laboratory method validation data were determined,and the calibration standard curves for 5 flavone aglycones were linear in the range of 0-10 g/kg with correlation coefficients more than 0995.The recoveries,at there spiked levels of 01,02,04 g/kg for quercetin and luteolin,005,01,02 g/kg for kaempferol,apigenin and baicalein after hydrolysis,ranged from 704%to 104%with relative standard deviations of 40%-12%.This method was suitable for the simultaneous determination and confirmation of flavone aglycones in Lonicerae Flos. |
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