Study On Quality Standard And Menthol Inclusion Process Of Banlan Qingre Granules

Objective:1The current quality standard is not perfect of Banlan qingre granules,so it is increased the content determination of metnthol and HPLC Fingerprint on the original quality standard basis.2Banlan qingre granules are composed of the Rhizoma et Radix Baphicacanthis Cusiae and menthol.Menthol unstable,volatile,so menthol inclusion process was studied to improve effectively menthol content and reliability.Methods:1(1)GC was used to determine the content of menthol in Banlan qingre granules.The chromatographic conditions were as follows:The PEG capillary column(30m × 0.32 mm × 0.25μm),the initial column temperature was 40℃,maintained for1 min,and rose to 80℃ at the rate of 5℃/min,finally rose to 120 ℃ at the rate of 3℃/min and maintained for 5min.The injection port temperature was 250℃.An FID was used as the detector and the temperature was 250℃.Split injection was performed with the diversion ratio of 10:1.(2)HPLC to establish the fingerprint analysis of Ban lan clear heat granule.chromatographic condition:Agilengt Zor Bax Eclipse XDB C18(4.6 mm×250mm,5um)with methanol~water solution as mobile phase in gradient elution mode at a flow rate of 1.0 ml/min.The determine wavelength was 250 nm,the temperature of column was 30℃ and the sample size was 10 ul.The similarity evaluation of common peaks were conducted by using the TCM Chromatographic Fingerprint Similarity Evaluation System(2012 edition).2By orthogonal experiment design,the compound was combined with beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin.The inclusionrate and inclusion yield of volatile oil were used as evaluation indexes,and select the best inclusion conditions and inclusion accessories.Results:1(1)The menthol sample showed a good linear relationship at the range of0.00536μg ~ 0.0536μg(r =0.99990).The average recovery rate was 99.55% and RSD was 1.45%(n=6).(2)We establish the HPLC fingerprints of ten bachs Banlan qingregranules.There were eight common peaks in HPLC chromatograms of ten batches of samples.The similarity of ten batches of samples were more than0.9.It was Accord with the similarity evaluation standard of Chinese medicine fingerprint.2The best inclusion accessorie is hydroxypropyl-beta-cyclodextrin,The optimum preparation condition was established as menthol:HP-β-CD1:8,HP-β-CD:water1:1,the inclusion temperature was 40℃,stirring for 3hours.Conclusion:1(1)The methodsare specificand simple with good reproducibility.They can be used for the quality control of Banlan qingre granules.(2)Thise method is simple,acurate,and reproducible,which can be used for the quality control and evaluation of Banlan qingre granules.2The process is stable,reasonable and feasible,it was improved effectively menthol content and reliability of Banlan qingre granules.