| Succinum is a kind of resin fossil Chinese medicine,which is irregular in shape of lump,bell emulsion and granular.Sometimes it contains fossils of plants or insects.Dispersed in coal or sandy clay.Generally from strata,clay,crisp,lighter body,called Succinum.The harder material extracted from the coal seam is called "coal percussion".Succinum mostly occurs in the clay,sand or coal seams of Late Paleozoic Carboniferous to Mesozoic Cretaceous and Cenozoic Tertiary,about 320 million years ago.Resins in Succinum mainly come from gymnosperms in paleontology,Pines and Cypresses.Ancient pines and cypresses were widely adapted to the plains and mountainous areas at different altitudes in temperate,cold and subtropical zones of the earth.Some of them could form coniferous forests in large areas,and fossils were formed after transformation over a long period of time.Succinum is produced in Fushun of Liaoning Province,Yongping,Baoshan and Lijiang of Yunnan Province,and Heilongjiang,Jilin,Xinjiang,Tibet,Shaanxi,Henan,Hubei and Sichuan.Among them,the output of Succinum is the highest and the quality is the best in Fushun Open-pit Coal Mine,Liaoning Province.Chinese medicine Succinum has a long history as a medicine.Some famous Chinese medicine prescriptions and Chinese patent medicines use Succinum as raw materials,such as Succinum Baolong pills,Succinum Huanjing pills,Qianlietong tablets,Succinum Anshen pills,Qingyu Pipi Zhedan,Lingbao Huxindan,Guanfang Zhibaosan,Ma Yinglong Musk Hemorrhoids Ointment,etc.However,the quality standard of Succinum is not perfect.Except for the 1977 edition of Chinese Pharmacopoeia,there is no national standard and the standard of Succinum contained in Hubei Pharmaceutical Standard.Theidentification methods of Succinum are scattered in various pharmaceutical works,mostly for the identification of characteristics and the physical and chemical identification methods for distinguishing rosin.Succinum is a kind of traditional Chinese medicine which is difficult to identify its origin from original plants,animals or minerals.Therefore,this study mainly focuses on the improvement of Succinum quality standards.Firstly,the origin,medicinal history and evolution of Succinum are sorted out and classified,and the appearances,physicochemical identification and other items of Succinum medicinal materials are supplemented.Through GC-MS technology,the compounds in Succinum are identified and compared,and the characteristic components in Succinum are determined.TLC method,infrared spectroscopy and other methods were used to identify Succinum,coal and adulterants.At the same time,near infrared spectroscopy and Raman spectroscopy were used to identify Succinum and its adulterants rapidly,which could provide reference for further improvement of Succinum quality standards,quality control of service drugs and development and utilization of Succinum medicines.Secondly,there is a certain controversy about whether coal Succinum can be used as Succinum medicinal.There is no coal Succinum in the National Compilation of Chinese Herbal Medicine,and it is stated in its notes that:"(coal Succinum)is mined from the coal seam.The body weight is hard,the color is black,the burning smoke is black and there is gas,which is different from the source of Succinum.It is not suitable for Succinum to be used as medicine.This study also makes a preliminary discussion on the medicinal basis of Meiper.Coal Succinum found in Fushun coal is one of the three major gemstone Succinum producing areas in the world and China(Myanmar,Baltic coast,Fushun).It has a long geological history.Although its texture is harder than Succinum,it chews crumbly and has no sandstone feeling.After treatment,the surface of coal Succinum has glass-like luster,which is similar to Succinum.However,through experimental study,it is found that coal Succinum is similar to Succinum in appearance and physicochemical characteristics.There are great differences between Succinum and Succinum in chemical composition.WhetherSuccinum can be used as an alternative is questionable.The main contents of this study are as follows:1.Systematic identification and comparison of Succinum and its common adulterants were carried out from its appearance,shape and physicochemical properties.Fire test and alcohol dissolution test were used for comprehensive determination,which enriched the content of physicochemical identification of Succinum and could be used for rapid and simple identification of authenticity and falsity of Succinum medicines.2.The fragrant tree essence in Succinum and olive resins was determined by GC-MS,and was verified by comparison of reference substances and FID detector.In the process of study,temperature programmed method was used to find that the high boiling point region had obvious characteristic absorption.The main structure of the substance was identified as beta-fragrant tree essence by mass spectrometry analysis,accompanied by other similar components.By analyzing several batches of Succinum samples,it was determined that the substance could be used as a characteristic of Succinum(Note: No detection in coal Succinum under the same chromatographic conditions).Secondly,it is the first time that this ingredient has been identified from Succinum.At present,there is no report on Succinum in domestic research papers.It was also found that there were beta-flavor tree essence in olive resin,one of the confusions of Succinum,but its relative content was different from other characteristic components.In the following quantitative analysis and pharmacological activity study of Succinum,comparative analysis could be carried out to further improve it.3.The fingerprints of low boiling point volatile components in Succinum and its adulterants were analyzed by GC-MS.It was found that the total ion flow patterns of Succinum samples from different sources were similar,and the relative contents of each characteristic component were comparatively consistent,and eight characteristic absorption were identified.The fingerprint characteristics of Succinum,coal,earth and olive resin samples were compared in the experiment.It was found that Succinum samples from different sourcesand batches had good consistency and obvious characteristics.There were significant differences between adulterants and counterfeit Succinum in chemical composition and relative content.And different batches are quite different.4.A TLC method was established for the identification of the characteristic component of Succinum,beta-fragrant tree essence.Succinum can be effectively distinguished from its adulterants and counterfeits by comparing the control materials with the control materials.The establishment of TLC method is based on the components of beta-fragrant tree essence determined by gas chromatography.According to the physicochemical properties of the ingredient,the preparation method of the sample and the solvent development system were optimized.The spots of TLC were clear and there was no interference.On this basis,the chromatographic differences of Succinum,Succinum,olive resin and rosin were compared and analyzed.The TLC method with the reference of Succinum and beta-fragrant tree was determined,which could be used as the quality control of Succinum.An important supplement to the system.5.Systematic identification of Succinum and its adulterants was studied by infrared spectroscopy.Because of the uneven texture of Succinum samples,if the simple diffuse reflection method may lead to the deviation and uncertainty of measurement,the samples were crushed in the experiment,and the feasibility of measuring infrared spectra by potassium bromide tablet method was studied.Through experiments,it was found that the infrared spectra of Succinum,coal Succinum and common confusions all have their own characteristics,from many batches of samples,different sampling time.It can be concluded from the comparative analysis that the spectra of different samples have obvious differences,and the infrared spectra of the same type of samples have good consistency.Through infrared spectrum analysis,the infrared characteristic absorption of Succinum and coal Succinum is summarized,which can be used as the identification basis of Succinum and coal Succinum commodities and their confusions.6.Qualitative identification and cluster analysis of Succinum and its adulterants werecarried out by using near infrared spectroscopy modeling analysis.The established method can effectively distinguish Succinum and its adulterants.Near Infrared Spectroscopy(NIRS)is a non-destructive and fast analysis method,which is widely used in the field of rapid detection.Its main principle is qualitative or quantitative analysis of substances by chemometrics and pattern recognition technology.Based on the above quality standard research,the model of Succinum sample is established and analyzed by OPUS software in the experiment,and the NIRS pretreatment method and characteristic spectrum are determined.In cluster analysis,all the samples of the same type,such as Succinum,olive resin,rosin and earthworm,are clustered into one group.Coal Succinum has independent characteristics,which are different from Succinum and other counterfeits.Similarly,in the qualitative model established by factor analysis,different samples have different distribution intervals in space,which can distinguish Succinum and its adulterants.To sum up,the physicochemical identification of Succinum was improved through systematic identification research,and the methods of infrared spectroscopy,TLC and GC-MS fingerprint were supplemented to provide reference for improving the quality standard of Succinum.The application of near infrared rapid detection method in the detection of Succinum medicinal materials in traditional Chinese medicine was studied and explored,which provided new ideas and methods for the identification of mineral medicines. |
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