| In this paper,the essential oil was extracted from fresh Cinnamomum pedunculatum leaves which was used as a raw material by using solvent-free microwave-assisted technology and compared with the traditional steam distillation method.The chemical composition and relative content of the essential oil of C.pedunculatum leaves obtained by different extraction methods were detected by GC-MS technology.Flavonols of myricetin,quercetin and kaempferol and proanthocyanidins were extracted from C.pedunculatum leaves by homogenate extraction technology under different technological conditions,which were optimized by the method of response surface method.Macroporous resin enrich and purify total flavonols and proanthocyanidins of the alcohol extraction.The main contents are as follows:The extraction of essential oil from C.pedunculatum leaves by the method of solvent-free microwave assisted,which was compared the traditional methods.We investigated the influence of microwave power and time,finally,we ascertained the best extraction conditions are 540 W of microwave irradiation power and 40 min of microwave irradiation time.The yield of essential oil is 6.50 ± 0.31 mL/kg.The operational conditions for GC-MS analysis was listed as follows:carrier gas(He)at a flow rate of 1 mL/min,injection volume 1 μL,split ratio 1:50,and injector temperature 270 ℃.The oven temperature was increased from 60 to 120 ℃ at a rate of 10 ℃/min,then increased to 200 ℃ at a rate of 10 ℃/min,and finally,to 280 ℃ at a rate of 10 ℃/min.The detector temperature and scan range were 280 ℃ and 15-500 atomic mass unit,respectively.To identify the compounds in the essential oils,the mass spectral fragmentation patterns were compared with those of similar compounds in a database of NIST05.The main components of the essential oil from C.pedunculatum leaves were borneol,cinnamyl acetate,eucalyptol,caryophyllene,and y-elemene etc.The flavonoids of myricetin,quercetin and kaempferol and proanthocyanidins were detected by high performance liquid phase whicn were extracted by homogenate technology from the residue with the essential oil has been extracted already.On the basis of single factor experiment,the extraction conditions were optimized by response surface method.The effects of homogenization time,liquid to material ratio and ethanol volume fraction on the yield of flavonols of myricetin,quercetin and kaempferol and proanthocyanidins were investigated.Finally,we determined the optimum extraction conditions were 4 min of the homogenate time,16:1 mL/g of the liquid material ratio and 71%of the volume fraction of ethanol.Under this condition,the content of flavonols and proanthocyanidins was 12.48 ± 0.57 mg/g and 71.97 ±2.71 mg/g,respectively.Set up HPLC method which was determinined the content of flavonols of myricetin,quercetin and kaempferol and proanthocyanidins.Chromatographic separation was carried out by a Kromasil-C18(5μm,4.6 mm × 250 mm)reversed-phase column,The proportion of mobile phase was methanol:water(0.5%phosphoric acid)= 50:50(v/v)and injection volume was 10 μL,the sample runs for 30 min at a flow rate of 1.0 mL/min at a temperature of 30 ℃.The UV detection wavelengths were set at 360 nm.Macroporous resin enrich and purify total flavonoids and proanthocyanidins of ethanol extraction were studied.By comparing 9 kinds of macroporous resin:HPD-80,D4020,X-5,HPD-400,HPD-450A,ADS-17,HPD-500 and HPD-600 to the ability of total flavonoids and proanthocyanidins.We believe that AB-8 is the ideal resin for the enrichment and purification of flavonoids and proanthocyanidins.The optimum adsorption and analytical parameters of the macroporous resin AB-8 were determined.The concentrations of flavonoids and proanthocyanidins were 0.79 mg/mL and 0.36 mg/mL and the optimum sample amount of 180 mL with a flow rate of 2 BV/h for dynamic adsorption.After the adsorption was completed,the elution was carried out with the volume fraction of 70%ethanol,and the flow rate was 1.5 BV/h.After purification,the purity of total flavonoids and proanthocyanidins were from 19.42%and 13.84%to 82.03%and 78.92%,respectively.Solvent free microwave-assisted was used to extract the essential oil from C.pedunculatum leaves and then the method of homogenate technology was used to break the plant cell wall of the surplus material,completelly.And by using macroporous resin enrich and separate target products to improve the purity.This method is rapid,effective and low cost.And this method had not been reported. |
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