The Research And Preparation Of The Control Extracts For The Identification Of Polygonum Multiflorum And Jujube Seed By Thin-layer Chromatography

Radix polygoni preparata(RPP)is the processed product of heshouwu,the dried root of polygonum multiflorum thumb.Modern chemistry and pharmacodynamics confirm that RPP contains three types of major active compounds:stilbene glucosides,anthraquinones and phospholipids.Semen zizyphi spinosae(SZS)is the dry mature seed of Ziziphus jujuba Mill.var.spinosa(Bunge)Hu ex H.F.Chou.Modern pharmacological studies have demonstrated that flavonoids,semen total saponins and jujube kernel oils from SZS are the main bioactive components.At present,the control herbs of RPP and SZS in the research and practical application have the following problems:SZS is more prone to rancidity beause it belongs to the seed herbs and contains abundant Fatty oil.RPP and heshouwu are processed by different methods and have different clinical usage,but their TLC identification methods are consistent in many standards,obviously which can not reflect the characteristics of processing method of TCM.The research topic is a part of the research project of "Chinese Pharmacopoeia"(2015 edtion)-"research and preparation of the control extract of crude drugs or decoction pieces appied to TLC".We take RPP and SZS as the object of study,use modern technology to preparate the extract in accordance with the principles and technical requirements of reference materials research,in conderation of their chemical composition and quality standards in current usage.Objective:Study the control extracts of RPP and SZS appied to TLC and preparate them.Then build the draft standards of control extracts.In addition,we amend the relevant quality standards.The research is important for the qualiy control and the safety of clinical utilization of TCM.Method:Review and summarize the chemical composition information system and usage in current standards of RPP and SZS.This provides theroretical basis and references for the further experimental design.We firstly collect four batches cude drugs of RPP and SZS,and screen out qualified medicinal materials from the samples as research targets by testing their qualities according to"Chinese Pharmacopoeia"(2010 edition).Through the experiment,the processes of extraction and preparation of the control extracts are set up,and determine process parameters,such as clearly extraction conditions(including the solvent,solvent concentration,solvent volume ratio,and extraction times etc.),the type and amount of excipients,the drying time,the yield of the control extracts.We study the Charactersitics,TLC behavior,content of active ingredients and moisture content of the control extracts to ensure quality.In order to know whether the extracts and the control crude drugs are in insistent with quantity and quality,we use a variety of different TLC conditions and methods of preparing the samples.We have a large-scale preparation of extracts,and examine their qualities each month.By the tests of stability,homogeneity,solubility,we define the factors affecting the stability,the kind of solvent to dissolve the control extracts and uniformity of content of the active ingredients.We develop the draft standards of control extracts of RPP and SZS.The main contents of the draft standards include name,origin,production method,characteristics,identification,specification,packaging,storage.We use the control extract instead of polygonum multiforum control crude drugs to identify RPP with TLC method in new quality standard of yangxueshengfa capsules.The control substances jujuboside A and B can be replaced with the control extract of SZS in the zaorenanshen particles and zaorenanshen capsules.Result:The result shows the sample PMRP-3 and ZPS-3 have good qualities and can be choosen as raw materials.The extraction and preparation process of the control extracts of RPP and SZS as follows:Pound the crude drugs of RPP into oedema powders.We extract chemical compositon of herbs by the heating reflux extraction.Reflux the crude drugs by Adding 10 times of 95%ethanol for 1 hours in the first time and Adding 8 times of 95%ethanol for 1 hours in the second time,then filter,merge the filtrate and Concentrate them to a modest degree(the relative density is about 1.0,(about 30℃)).Add 2.2 times amount of dextrin,the dry particles are got after the procession of squeezing through a 20 mesh sieve and drying for 5 hours.The extract yield of RPP was 36.4%Pound the crude drugs of SZS into oedema powders.We extract chemical compositon of herbs by the heating reflux extraction.Reflux the crude drugs by Adding 10 times of 95%ethanol for 1 hours in the first time and Adding 8 times of 95%ethanol for 1 hours in the second time,then filter,merge the filtrate and Concentrate them to a modest degree.Add 2 times amount of dextrin,the dry particles are got after the procession of squeezing through a 20 mesh sieve and drying for 5 hours.The extract yield of SZS was 74.2%.The quality stability of extracts of both RPP and SZS are mainly affected by the humidity factor,therefore,they should be placed in a closed,cold and dry environment.We have amended original standards of TLC identification for SZS.We establish the quality standards of the control extacts appied to the TLC of RPP and SZS.We have amended original standards of the zaorenanshen particles,zaorenanshen capsules and capsules.Conclusion:In summary,the extraction and preparation process of the control extracts we have studied are feasible.The control extracts have superior qualities,stable physical and chemical properties,good content uniformity and simple preparation of sample.Therefore,it could be used as a standard substance.Studying on the control extracts has a important theroretical significance and application value.