| ObjectiveTo researching on processing technology (Softening process, Drying technology)and quality standards of exocarpium decocting pieces by the use of modern analytical technology like UPLC method, high performance liquid chromatography (HPLC), Ultraviolet spectrophotometry, The method of ammonia cause cough, DPPH method, establish normative processing technology and quality standards of exocarpium decocting pieces. Provide The scientific basis about Standardization drug use and Quality control of exocarpium and its Processed products.MethodsThe content of total flavonoid was determined by Ultraviolet spectrophotometry, The content of naringin and rhoifolin was determined by UPLC. The fingerprints of exocarpium was studied by HPLC. Pharmacodynamics study by The method of ammonia cause cough、DPPH method、pyrogallicacid method and Salicylic acid method.optimize the Softening process and Drying technology of exocarpium by response surface design and orthogonal design. Determine moisture content、Ash content and Extract content of exocarpium decocting pieces according of the method in ChP.2010. Vol I.Result1Study on the Softening process of exocarpium decocting piecesThe experiment select the method of water embellish under reduced pressure、Steamed、stuffy embellish.According to the softening method in documents and The experimental results,get Specific operating mode of three kinds of softening method. The flavonoids, naringin, rhoifolin and naphtha as a nucleoside complete index, through comprehensive pointrating method select the best way to soften exocarpium, results of Total score calculation shown:steam method> water embellish under reduced pressure method> stuffy embellish method> Medicinal materials. Steam method and water embellish under reduced pressure method get similar results, Steam method has the advantages of concise, time-saving, water-soluble ingredients small loss, So the experiment choice steam method for the best softening method. By response surface design,to optimize process parameter of steam method.the process parameter of steam method should be:select steam method, Steamed time (8h), steamed temperature(50℃).Through verification experiment, the results of the index component content of steamed sample improve significantly higher than stuffy embellish, in concluded that the method is Practical and feasible.2Study on the Drying technology of exocarpium decocting piecesThe experiment select the method of constant temperature drying, vacuum drying, microwave drying. through comprehensive pointrating method select the best way to soften exocarpium is vacuum drying method and microwave drying method, the two-method get similar results, but the microwave drying method has thethe advantages of processing fast、time-saving、high thermal efficient、 high-quality、high-quality, etc. So the experiment choice smicrowave drying method for the best Drying technology of exocarpium decocting pieces.By orthogonal design, to optimize process parameter of microwave drying method. The experimental results show that the process parameter of microwave drying method should be:Medicinal materials(30g), time(12min),Microwave: light waves (49%:51%). Through verification experiment, the results of the index component content of microwave drying sample improve significantly higher than constant temperature drying sample, in concluded that the method is Practical and feasible.3Study on the quality standards of exocarpium decocting pieces3.1the result of slices Checkin the20samples of exocarpium decocting pieces, Range of water content is7.84%～8.98%, the average content is8.46%; Range of total ash content is2.50%～4.21%, Average is3.51%;Range of Acid-Indiscerptible Ash Content at0.03%～0.23%, the average content is0.10%, Acid-Indiscerptible Ash Content in Different varieties of tangerine Are very different. 3.2Extraction ContentDetermination result of Extraction Content about20samples of exocarpium decocting pieces show that range of Water-Solubility Maceration Extraction Content (WSMEC) by method of hot-maceration is35.47%～51.27%, the average content is44.59%. Range of Ethanol-Solubility Maceration Extraction Content (ESMEC) by method of hot-maceration is19.68%～29.48%, the average content is24.67%.3.3Index Ingredients DeterminationDetermination result of Extraction Content about20samples of exocarpium decocting pieces show that Index Ingredients in Different varieties of exocarpium decocting pieces Are very different. Range of The flavonoids is99.77mg/g～264.96mg/g, Range of naringin is72.13mg/g～205.22mg/g, Range of rhoifolin is3.18mg/g～17.72mg/g, Range of naringin:The flavonoids is65.90%～85.91%, Range of rhoifolin:The flavonoids is1.93%～9.94%.3.4HPLC fingerprint of exocarpium decocting piecesMatching the peaks of20sample fingerprints, wo get23peaks owned by both, The large area for peak one by one is peak naringin, peak rhoifolin, peak naringenin. The external appearance of each sample’s HPLC fingerprint is very alike, The data analysis showed that19peaks owned by both in totally peaks, having90%area above. The fingerprint similar degree is very high at the same time, all big in0.95.4Study on Pharmacodynamics of exocarpiumAntitussive research shows,1、Cough time:Except low-dose group before processing Can not extend cough latency period of mice (P>0.05), The rest of the group all can extend cough incubation period of mice(P<0.05or P <0.01),The same is low dose group,No significant difference between before and after processing, The same is high dose group, Before and after processing are significantly different (P<0.05), Processing (steamed) samples make Cough time of mice extend57.6%;2、Cough number:No matter whether or not be processing, exocarpium can reduced the mice cough number in2min(P<0.01),After processing (steamed), cough rate of Low dose group reduced by27.4%, cough rate of high dose group reduced by46.5%, All has significant difference (P<0.05).Antioxidant experimental results showed, The flavonoids content is higher, oxidation resistance, the better, exocarpium after processing (steamed) and exocarpium beforer processing compared, The flavonoids content increased, antioxidant ability enhancement。Exocarpium compared with light exocarpium, The flavonoids content increased, antioxidant ability enhancement.Conclusion1By response surface design, to optimize process parameter of steam method. the process parameter of steam method should be:select steam method, Steamed time (8h), steamed temperature(50℃)2By orthogonal design, to optimize process parameter of microwave drying method. The experimental results show that the process parameter of microwave drying method should be:Medicinal materials(30g), time(12min),Microwave: light waves(49%:51%).3on the basis of the experimental results, establish preliminary quality standards of exocarpium decocting pieces:water content of exocarpium decocting pieces must be no more than10%; total ash content must be no more than5.0%; Acid-Indiscerptible Ash Content must be no more than0.3%; Water-Solubility Maceration Extraction Content(WSMEC) must be not less than32.0%, Ethanol-Solubility Maceration Extraction Content(ESMEC)must be not less than18.0%; Calculated on the anhydrous substance, The flavonoids content may not be less than90.00mg/g, naringin content may not be less than65.00mg/g. rhoifolin contentmay not be less than3.00mg/g.4Establish preliminary HPLC fingerprint of exocarpium decocting pieces. The fingerprint similar degree is more than0.95,23common peak area compared with the total peak area, having90%area above. We could make use of it to have mode the initial establishment t of characteristic fingerprint diagram with the decocting pieces of Citri Grandis. That would help it’s production developing to the modernized, standardize direction.5exocarpium after processing (steamed), Antitussive effect and antioxidant effect all have been improved greatly, the change of pesticide effect And The flavonoids content Are related, provide the evidence for accurate, effective of exocarpium clinical treatment and Clarify processing mechanism of exocarpium decocting pieces. |
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