| The Chinese Pharmacopoeia(2015 Edition)stipulates that the plant is Paris polyphylla Smith var.yunnanensis Franch.Or Paris polyphylla Smith var.chinensis.which belongs to the family Liliaceae.Hand.-Mazz.The dry rhizome of Paris was first contained in "Shennong Herbal Classic" in Han Dynasty.It was classified as the lower grade,its taste was bitter,its property was slightly cold,and it had a small poison,which belonged to the liver channel.Mainly used for epilepsy,shake head tongue,the next three insects,snake venom and other diseases.It has a long history of clinical application,remarkable effect and wide clinical application.Due to the exhaustion of wild resources,the difficulty of artificial cultivation and the long time of cultivation,the market gap has been enlarged.In order to make rational use of resources and maintain the normal circulation order of the market,this paper studies the producing area processing,processing technology,quality status and grading standard of heavy building.Objective:1.Collection all country of the paris pieces,with appearance and inner component content index as the indexs,assess the quality of commercial the paris,and establishment the paris decoction pieces quality standards.2.To optimize the processing technology of fresh paris and the processing technology of the paris medicinal slices with the appearance and index component content.3.Using liquid chromatography-mass spectrometry technology combined with multivariate statistical analysis method distinguishes different drying methods and drying temperature of the sample.The influence of different drying process of samples internal components is clarified.4.According to the content of appearance and index components,the grading standard of the paris medicinal slices was divided,and the grading standard was established.Methods:1.Collection all country of the paris medicinal slices.In the aspect of evaluation of appearance characters,the relative indexes of the outer epidermis color,section color,texture and diameter of the heavy building were measured.In the aspect of content evaluation of intrinsic index components,the method of characteristic atlas of the paris was established by high performance liquid chromatography(HPLC),and the nine indexes component content determination method of Polyphyllin Ⅶ,Ⅵ,Ⅴ,Ⅶ Ⅱ,Ⅰ,H,Dioscin and Gracillin were established.And the determination of extract content in the paris was established.The total ash,acid insoluble ash and water content limit were determined according to the general rules 2302 and 0832 of the fourth part of the Chinese Pharmacopoeia(2015 edition).Combined with the results of appearance characters,content of intrinsic index components and relevant inspection items,the quality status of the pieces sold in the market was evaluated.2.The processing technology of fresh Paris polyphylla.By measuring the appearance characters and the content of 9 index components of the samples prepared under different drying conditions,the drying technology of fresh Paris polyphylla was selected.The processing technology of Paris polyphylla pieces was optimized by investigating the moistening process,cutting process and drying process,and the optimum processing technology of heavy building pieces was finally optimized.3.The difference of internal components between freeze-drying and blow-drying samples was studied by means of liquid chromatography-mass spectrometry technology combined with multivariate statistical analysis method,and the effect of drying method on chemical composition was clarified.The internal composition differences of samples prepared at different drying temperatures under blast drying method were studied by means of liquid chromatography-mass spectrometry technology combined with multivariate statistical analysis method,and the effects of temperature on chemical composition of Paris polyphylla under blast drying method were clarified.4.By measuring the appearance character and intrinsic index component content of the Paris polyphylla pieces sold in the market,grading the Paris polyphylla pieces and establishing the classification standard of the Paris polyphylla pieces are established.Results:1.31 batches of the Paris polyphylla pieces were collected,including 18 batches from Yunnan province,10 batches from Sichuan province,and 1 batches from Guizhou,Henan and Hubei provinces.In the aspect of evaluation of appearance characters,the color of the outer epidermis were all in line with the relevant regulations of Chinese Pharmacopoeia(2015 Edition),and the section color identified Yunnan 5 as the counterfeit of Polygonum bistorta L.,and other batches of samples conforming to the regulations of the Pharmacopoeia.In Yunnan 4,Yunnan 11,Yunnan 12,Sichuan 2,Sichuan 5 and Henan 1,the whole diameter of the Paris polyphylla pieces was less than 1.0 cm.31.The thickness of the Paris polyphylla pieces sold on the market was larger than that of the Chinese Pharmacopoeia(2015 Edition).In terms of evaluation of intrinsic index components,a method was established for the determination of the contents of thermal alcohol-soluble extracts in the Paris polyphylla pieces.The contents of extracts were in the range of 31.98～8.98%(mean value was 17.44),and the average content of extracts from Yunnan was 16.7%.The average content of extracts from Sichuan was 17.8.The results showed that there was great difference between the contents of extracts from Zhonglou and Yunnan Province,and the average content of extracts from Yunnan was slightly lower than that from Sichuan.The method of characteristic map was established,and 9 peaks were used as target peaks for methodological investigation.The RSD values of precision,repeatability and stability were all less than 3.0%,which was in accordance with the relevant regulations of methodological investigation.The chemical composition of different batches of the Paris polyphylla pieces was different from each other and the similarity was low.A method for the determination of the content of nine index components was established.The RSD values of precision,repeatability and stability were all less than 3.0%,The recoveries of each index component were between 95 and 105%.The linear relationship of the contents of nine index components was all higher than 0.999 in a certain range.The Polyphyllin Ⅰ,Ⅱ,Ⅵ,Ⅶ total content of Yunnan7,Yunnan 10,Yunnan 11,Yunnan 12,sichuan 3,sichuan 10 and guizhou 7 less than 0.6%,in addition to the above batchs the paris pieces’s 9 kinds componts total conent is between 1.09%and 6.64%.In terms of related inspection items,The total ash content of Yunnan 12 batche samples is more than 6.0,the total ash content,acid insoluble ash and moisture content of other batches are all in accordance with the regulations.By comparing the appearance characters,the content of index components and the test results of relative inspection items of the Paris polyphylla pieces sold in market,It was found that the average value of the total content of 9 components in the samples from Sichuan province was higher than that of the samples from Yunnan province.There were 11 unqualified samples in the 31 samples sold in the market,38.7%of which were counterfeit or unqualified products.There are hidden dangers in the quality of the pieces sold in the Paris polyphylla market.2.The fresh paris polyphylla’s origin processing craft.appearance evaluation,dried in the sun samples,drum wind drying 50℃,65℃ drying the sample appearance accord with pharmacopoeia requirements.Freeze-dried samples are large in volume,crisp and powdery,with a basic appearance of fresh herbs.the 80℃ drum wind drying herbs crispy texture,section brownish red to brown,do not conform to the requirements of the pharmacopoeia.Inner index composition evaluation,by comparing the different process dry samples of 9 kinds of saponins content,found that 50,65℃ drum wind drying way sample preparation time is short,9 kind of component content is higher,so the best paris polyphylla’s origin processing craft is drum wind drying temperature is 50～65℃,processing time is about 4 days,stay to the moisture content is less than 12%.Processing technology of the paris polyphylla.In the process of moistening,sprinkling water on the medicinal materials for the first time accounts for 65～75%of the quality of the medicinal material,covering the wet gauze,and then sprinkling the water with the quality of 5%of the medicinal materials every 12 h,and turning the medicinal materials at the same time,moistening for 3 days or so,and the softening of the medicinal materials,suitable for cutting and drying.The rate of abortion was low in thick slices.Drying process optimization,50℃,65℃,80℃ drying sample appearance all conform to the requirements of the pharmacopoeia,the colloid pieces rate of 80℃ drying sample is greater than the other samples.Comparing different temperature drying pieces’s nine indexes component content,found that 50,65℃ dry sample content is higher.Comprehensive appearance index,and nine kinds of indexes component content,the best drying temperature is 50～65℃.The best processing technology,sprinkling water on the medicinal materials for the first time accounts for 65～75%of the quality of the medicinal material,covering the wet gauze,and then sprinkling the water with the quality of 5%of the medicinal materials every 12 h,and turning the medicinal materials at the same time,moistening for 3 days or so,waiting for the medicinal material to be completely softened.Under the condition of thick slice,blast drying temperature 50～65℃,the moisture content of the slice is less than 12%.3.The composition difference of heavy tower in different processing process was elucidated by means of liquid chromatography-mass spectrometry technology combined with multivariate statistical analysis methods.In different drying methods,the content of proto-dioscin,parisaponin I,proto-gracillin was higher in freeze-dried samples,and the content of Reclinatoside in blast drying was higher.The content of Proto-dioscin,Dichotomin,parisaponin I,Proto-gracillin in the samples of the paris polyphylla at different drying temperatures was higher than that in the samples r dried at 65℃.The content of kaempferol was higher in the samples of heavy tower dried at 65℃.4.The contents of external appearance and intrinsic index components of 30 batches pieces sold in the market and 12 batches of self-made pieces were determined.According to the measured data,the pieces were divided into three grades.A grade Polyphylla pieces,The diameters of pieces should not be less than 1.4 cm;the outer epidermis should be yellowish brown or grayish brown.The total content of the saponins Ⅰ,Ⅱ and Ⅶ should not be less than 1.5%;the water content should not exceed 12%;the total ash content should not exceed 6.0%;the acid insoluble ash should not exceed 3.0%.The second grade Polyphylla pieces,The diameters of pieces should not be less than 1.2cm;the outer epidermis should be yellowish brown or grayish brown.The total content of the saponins Ⅰ,Ⅱ and Ⅶ should not be less than 0.9%;the water content should not exceed 12%;the total ash content should not exceed 6.0%;the acid insoluble ash should not exceed 3.0%.The third grade Polyphylla pieces,The diameters of pieces should not be less than 1.0 cm;the outer epidermis should be yellowish brown or grayish brown.The total content of the saponins Ⅰ,Ⅱ and Ⅶ should not be less than 0.45%;the water content should not exceed 12%;the total ash content should not exceed 6.0%;the acid insoluble ash should not exceed 3.0%.Conclusion:1.The method of characteristic atlas of the paris Polyphylla pieces was established in this experiment.9 kinds of index component content detection methods and the determination method of thermal alcohol soluble extract content of heavy tower can be accurate,which can steadily reflect the difference of intrinsic index component content of different batches.Combined with the examination of the related indexes of the appearance characters of the paris Polyphylla pieces,the quality situation of the pieces sold on the market can be fully reflected.Among the 31 batches of the pieces sold in the market,there are 11 unqualified products,of which 38.7%are counterfeit or unqualified products.There are hidden dangers in the quality of the pieces sold in the heavy building market.2.The processing technology of fresh medicinal materials and the processing technology of paris medicinal slices have great stability that can be used for the processing and production.3.Different drying methods and different temperature drying samples were studied by means of liquid chromatography-mass spectrometry technology combined with multivariate statistical analysis methods,and the differences of chemical components in different drying methods and different temperature drying samples were discussed.The higher temperature,the more related components of the hydrolysis.4.The standard of grade division of pieces has stipulated the diameters and the content of internal index components of the paris medicinal slices.This standard is simple and easy to operate,and can be used to divide the different quality the paris medicinal slices well. |
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