Study On The Extraction And Determination Of Volatile Oil In Ganmaoqingre Granule

Ganmao Qingre granules composed of11herbs, mint,schizonepetaspike,Saposhnikovia divaricata, bupleurum root, perilla leaf, the root ofkudzu vine,Platycodon grandiflorum, bitter almond, angelica,corydalis, reedrhizome.It is considered to have a good effect on the cold cold-inducedheadache, fever, chills, body ache, cough and throat and other symptoms. It isrecorded in the "people’s Republic of China Pharmacopoeia"2010Edition (a).Studies have shown that, the volatile constituents are the main effectivepart of Ganmaoqingre granules treating cold, anti-inflammatory, antibacterialand antiviral,antipyretic, antitussive effect.The provisions ChinesePharmacopoeia standards, schizonepeta spike, mint, basil essential oilcomponents need to be extracted.At present, the volatile oil extractiontechnology of the product is the distillation method, there is the problemoflong extraction time, extraction efficiency is low, and there is no contentcontrol.In order to improve the cold heat granules volatile oilextractiontechnology level and quality level of control.I conducted this study.Objective:1.To study and formulate Ganmao Qingre granules volatile oil extractionprocess.2.Establish a GC method to determin three active constituents of thevolatile oil in Ganmaoqingre granule once, including Menthol, Pulegone andPerillaldehyde.Methods:1.Study on extraction process of volatile oil in Ganmaoqingre granule Put the amount of oil as the evaluation index to optimize the extractionmethod. By comparison, Jing Jiesui mint,basil leaves three herbs alone toextract volatile oil and mixed extract volatile oil.The amount of oil as theevaluation index to ascertain extraction technology, through the comparisonofdistillation (SD) and distillation distillation coupling (WER)of two kinds ofvolatile oil extraction process.Through the combination of water, soaking time, extraction time threefactors of different levels of study, orthogonal experimental design, with theamount of oil as the evaluation index, preferably with WER process mixture toextract volatile oil.And through experimental verification and amplificationexperiments, prove that the method is reproducible and process maturity.In theorthogonal test, determination of the content of menthol, pulegone, and perillaaldehyde in volatile oil,evaluation of different process parameters on the effectofvarious components of essential oil.2.Method for determination of menthol, pulegone, perilla aldehyde in thevolatile oil in Ganmaoqingre granulesUsing gas chromatography (GC) method, based on gas chromatographycolumn type, temperature programmed selection of conditions, internalstandard, determined to meet the requirements of the chromatographicconditions.Methodological study by specificity test,precision test,repeatability,stability test, recovery test, the linear range test.By testing five batches of samples, which are proved feasible method forthe content determination.Results:1.According to the three kinds of medicine separate extraction oil6h,according to the prescription ratio calculation of mixed extraction volume ofvolatile oil, WER method and SD method are2.43mL and2.12mL; three herbsmixed extraction6h, WER method and SD method were2.88and2.95mL.Visible, the extraction of volatile oil in Ganmaoqingre granules, by using threekinds of herbs mixed extraction is appropriate, and the WER was better than SD.2.Orthogonal experimental results show that the extraction of volatile oil,influence factors of WER Technology: extraction time> soaking time> theamount of water, preferably the best extraction process parameter is A3B2C2,which is7times of water, soaking90min, extraction3h.3.Experiment and enlarged experiments, results showed that theextraction of volatile oil, Ganmao Qingre granules by WER technology, isreproducible, mature technology, has a good industrial prospect ofimplementation.4. The sample is separated on a column of DM-FFAP（30m×0.25mm×0.25μm）, and detected by FID, the carrier gas is N2,the speed of flowis1mL/min; the temperature of injector and detector is250℃；thetemperature of column is from120℃and then heating up to140℃by2℃/min；and continue heating up to220℃by15℃/min，and keep5minutes, the sample size is1μL and the split ratio is20:1. Menthol iscalculated according to the number of theoretical plates should not be less than110,000, menthol, pulegone, respectively perillaldehyde other adjacent peakseparation is greater than1.5.5.Through the study, the content determination method is specific,menthol(in the34.034~343.04g/mL range), pulegone(in the88.998~889.98g/mL range), perilla aldehyde(in the19.2636~192.636g/mLrange) respectively, there was a good linear relationship. Good precisioninstrument, RSD of peak area values were: Menthol0.88%, pulegone0.97%,perillaldehyde0.97%. The test solution of menthol, pulegone, perilla aldehyde24h at room temperature is stable. Experimental good reproducibility, menthol,pulegone, perillaldehyde RSD values were0.74%,0.61%,1.66%. The averagerecovery of menthol and pulegone and perilla aldehyde rate was99%,102.13%,97.46%, RSD respectively:1.81%,1.71%,1.87%.6.Through the verification of the5batch of volatile oil samples, provedthis method is suitable for the corresponding testing requirements. Conclusion:Through this research, developed a new extraction technology of volatileoil in Ganmao Qingre granules by WER.Process parameters are as follows:first crushing herbs, then according to the proportion of prescriptions toweighing, mixing, using the method of WER, adding7times water, soak90min, extraction3H.In the new process(WER) and the traditional process(SD)comparison,Basically the same in the oil amount, extraction time isdecreased from5h to3h, have obvious advantages.The GC method this research establishment, determination the contentsof menthol and pulegone and perilla aldehyde in volatile oil of Ganmaoqingregranules.Simple and quick, specific, high precision, reproducibility, goodstability, good linearity, recoveries qualified.The three components in thevolatile oil can pass through a sample detected.Can be used for quality controlof volatile oil of cold heat particles, to ensure product quality to ensure that theclinical efficacy of practical significance...