Studies On Chemical Components And Method Of Quality Assessment Of Bichengqie

Litsea cubeba(Lour.)Pers.was derived from the ripe and dried fruitage..It has been recorded in the edition 2005 of Pharmacopoeia of the PRC for warming and dispersing coldness as well as relieving pain.14 Litsea cubeba(Lour.)Pers samples were collected from different habitats,which are used for the studies on the chemical components and the method of quality assessment.The chemical compositions of essential oil from Litsea cubeba(Lour.)Pers have been studied by GC-MS method.36 constituents of essential oil were got and 32 of them were identifed.The total content of the identified compounds was 98.0%.The chemical compositions of fatty oil from Litsea cubeba(Lour.)Pers have been studied by GC-MS and known substance reference methods.14 fatty acid compounds were got and 11 of them were identifed.The total content of the fatty acids was 82.9%and the unsaured fatty acids was 55.9%.The content of linoleic acid was the highest(13.5%)and geranic acid is the next(13.1%).Capillary Gas Chromatography(CGC)method was established for the simultaneous determination of four major components,namely 6-Methyl-5-hepten-2-one,limonene,linalool and citral in essential oil from Litsea cubeba(Lour.)Pers.The CGC analysis was performed on a 30 m×0.50 mm i.d.SE-54 capillary column,and was carried out with temperature programs. Split radio 1:1,The orthogonal design was adopted to optimize the extraction of 6-Methyl-5-hepten-2-one,limonene,linalool and citral,The optimal extracting condition was ten fold distilled water the amount of material,oaked for 5 hours,refluxed for 6 hours each time. The good linear regression relationship was obtained over the range of 0.03004～1.502 mg·ml^-1 (r=0.9999)for 6-Methyl-5-hepten-2-one,0.01788～0.894 mg·ml^-1(r=0.9997)for Limonene,0.01618～0.809 mg·ml^-1(r = 0.9997)for Linalool,0.07924～3.962 mg·ml^-1(r= 0.9999)for citral,The average recoveries were 101.5%(RSD = 2.1%),96.9%(RSD = 3.0%), 99.6%(RSD = 3.6%),98.6%(RSD = 4.3%),respectively.The assay method is simple,rapid, reliable and reproducible and provide a quantitative basis for the quality assessment of Bichengqie.A capillary gas chromatographic(CGC)method equipped with flame ionization detection was developed for the simultaneous analysis of palmitic acid,oleic acid and linoleic acid in Litsea cubeba(Lour.)Pers.Compounds were separated on an Agilent DB-17 capillary column (30 m×0.25 mm i.d,0.25μm).The polar column was 170℃programmed to 250℃at 5℃·min^-1for 10 min.Split radio,10:1;detector temperature,250℃.The orthogonal design was adopted to optimize the derivation reaction conditions of fatty oil.The optimal derivatization conditions of fatty oil were described as follows:sample was dissolved in 5 ml of a 0.5%w/v solution of sodium hydroxide in methanol in a 25 ml flask with a ground-glass stopper and boil under a reflux condenser for 45 min.Add 2.0 ml boron trifluoride-ether solution through the condenser and boil for 5 min.Palmitic acid showed a good linear relationship in the range of 0.04000～0.4000 mg·mL^-1(r = 0.999 5)and the average recovery(n = 3)was 100.0%,RSD was 1.7%;oleic acid showed a good linear relationship in the range of 0.06672～0.5838 mg·mL^-1(r = 0.999 9)and the average recovery(n = 3)was 100.4%,RSD was 2.9%;Linoleic acid showed a good linear relationship in the range of 0.0994～0.869 mg·mL^-1(r = 0.999 7) and the average recovery(n = 3)was 97.2%,RSD was 0.7%.The assay method is simple, rapid,reliable and reproducible and provide a quantitative basis for the quality assessment of Bichengqie.GC fingerprint chromatogram was established for essential oil from Litsea cubeba(Lour.) Pers..The analyses were performed on a Shimadzu 2010 Gas Chromatograghy(GC)system equipped with FID detector.Separation was carded out on DB-Wax capillary column(30 m×0.25 mm i.d,0.25 pan).The non-polar was 50℃programmed to 75℃at 3℃·min^-1,then to 130℃at 10℃·min^-1,and then to 240℃at 5℃·min^-1for 15 min;Split injection was conducted with split radio of 10:1 detector temperature,250℃.14 batches of Litsea cubeba(Lour.)Pers.were studied under this condition.With the Ward's method and the Squared Euclidean distance used as the measurement index,the Hierarchical cluster was applied to the fingerprints of Litsea cubeba(Lour.)Pers.and the 14 batches of Litsea cubeba(Lour.)Pers.was divided into two grades.Among them the gradeⅠwas commendatory and the gradeⅡwas general.Mutual pattern was established from 12 batches in the gradeⅠ.Similarity calculations were studied by comparing the GC fingerprint chromatograms of Litsea cubeba(Lour.)Pers.and mutual pattern. The similarity by the Euclidean distance,Pearson correlation,Cosine was calculated respectively.These results of the commendatory should be all over 0.90 and the other samples were the general.The method can be used as a quality control method for Litsea cubeba(Lour.) Pers.