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Extraction, Separation And Preliminary Research Of Chemical Compositions In Loropetalum Chinensis (R. Brown) Oliv

Posted on:2010-04-19Degree:MasterType:Thesis
Country:ChinaCandidate:L Q YouFull Text:PDF
GTID:2144360275490516Subject:Chemical Biology
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Loropetalum chinensis(R.Brown) Oliv.,called"Ji Mu",is an important folk medicinal resources with the efficacy of hemostasis,anti diarrhea,acesodyne and so on.In this study,the extraction,isolation,purification,structure identification, determination,infuse conditions of the chemical compositions from Loropetalum chinensis(R.Brown) Oliv.were studied.In this study,the extract method was adopted to extract the chemical compositions from Loropetalum chinensis(R.Brown) Oliv..Then extraction method and chromatography were used to isolate and purify the crude extracts(462 g).Eight compounds were got from the column chromatography of Macroporous Adsorption Resin,polyamide resin,silica gel,ODS,Sephadex LH-20 and Toyopeal HW-40C. According to their melting points,color reactions and other physical and chemical properties and data of their NMR(1H-NMR,13C-NMR),their structures can be identified:Kaempferol(C15H10O6,256.1 mg,2.8×10-3%),Quercetin(C15H10O7,71.6 mg,8.0×10-4%),the mixture of myricetin-3-O-β-D-glucoside and myricetin-3-O-β-D-galactoside (59.7 mg,6.6×10-4%),myricetin-3-O-α-L-rhamnoside(6.0 mg, 6.7×10-5%),the mixture of quercetin-3-O-β-D-glucoside and quercetin-3-O-β-D-galactoside (150.0 mg,1.7×10-3%),kaempferol-3-O-β-D-galactoside(5.9 mg, 6.6×10-5%),kaempferol-3-O-β-D-glucoside(8.1 mg,0.9×10-4%).A method based on reversed phase high performance liquid chromatography was developed to simultaneously determine the content of Quercetin,Kaempferol and Myricetin in the Loropetalum chinense(R.Brown) Oliv..Test solution was prepared by one hour's refluxing extraction with 80%methanol and 30 min's hydrolysis with 5%hydrochloric acid.UltimateTM XB-C18(150 mm×4.6 mm,5μm) column was used and eluted at 25℃with a mobile phase of acetonitrile and 0.4%phosphoric acid(32:68,v/v) at a flow rate of 1.0 mL/min.The calibration curves were constructed between peak area measured at 360 nm and the injected quantity,giving a linear working rang of 0.072 - 2.16(μg)(R2=0.9999) for all the three analytes.The spiked recoveries(n=6) were 99.1%,97.0%and 97.9%with RSD of 1.45%,1.38% and 2.04%,respectively.This method is considered to be stable,accurate, reproducible and suitable for quality control of Loropetalum chinense(R.Brown) Oliv..We also studied the infuse conditions of Loropetalum chinensis(R.Brown) Oliv. by orthogonal experiment.We studied three factors from two different solvents (ethanol and acetone):solvent concentration(solvent:H2O),wieght than solution (WTS,g/mL) and soaking time(h).Every factor was studied by 3 conditions with the use of L9(34) form.The optimum conditions of extraction is that the raw material was soaked in 50%(v/v) acetone-water solution 10 times as many as its weight for 24 h. And the factor which has greatest impact on extractive quantity is solvent concentration,followed by the WTS,and finally soaking time.
Keywords/Search Tags:Loropetalum chinensis (R. Brown) Oliv., Extraction and isolation, Structure identification, Content mensuration, Orthogonal design
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