Extraction And Analysis Of Flavones In Cauline Vegetables

In this paper, a method of extraction and purification of flavones in celery and Broccoli using accelerated solvent extraction (ASE) and macroporous resin had been established. And the separation and identification of the flavones was performed through high performance liquid chromatography electrospray ionization ion trap multistage mass spectrometry (HPLC-ESI-MS").The single factor experiment and orthogonal analysis were used to optimize the extraction conditions, the best parameters were as follow:preheating time:5 min; static extraction time:5 min; extraction pressure:10.3 MPa; extraction temperature:90℃; ethanol concentration:80%; flush volume:60%; N2 purging time:60 s; cycle index:3.The purification process of celery flavones was also studied. Four different macroporous resins (AB-8, D101, D4020, NKA-9) were evaluated by the adsorption and desorption properties for celery flavones. Among them, the type D101 macroporous resin was chosen for purify celery flavones.The process conditions were as follow:the proportion of flavones and the dry resin 1.4 mg/g, the eluent:80% ethanol water solution, the elution volume:4BV.The instrument parameters of HPLC-ESI-MS" were optimized to separate and identity the flavones. The column:ZORBAX Eclipse XDB-C18(2.1 mm×150 mm,3.5 μm Agilent); column temperature:40 ℃; flow rate:0.2 mL/min; mobile phase:methanol (B) and water which containing 0.1% formic acid (A), the gradient elution conditions:0-20 min 20%-30% B; 20-30 min 30%-40% B; 30-55 min 40%-55% B; 55-65 min55% B; 65-66 min 55%-20% B; 66-76 min 20% B, diode array detector(PDA) scan wavelength:230-500 nm; capillary temperature:300 ℃, capillary voltage:-15 V; spray voltage:4.5 kV; sheath gass flow rate: 30 arb; sweep gass flow rate:5 arb.The total flavones yields under these conditions in celery leaves, celery stems and broccoli leaves were 14.53 mg/g,1.80 mg/g and 6.35 mg/g, respectively. The purity of flavone in powder purified by macroporous resins was 66.42%, and the purity of flavone in powder without purification was 25.03%. The recovery was ranging from 95% to 108%. According to the HPLC retention time, fragmentation patterns of standard materials, and MS" fragmentations, a total of 14 flavones in celery and 9 flavones in broccoli had been identified. These results provide the theoretical support for further processing of celery and broccoli.