| Objective:The pearl stratum powder is dried fine powder made from the shells of Hyriopsis cumingii(Lea)or Cristaria plicata(Leach)or Pteria martensii(Dunker),which remove the cuticle and prism layers.Hyriopsis cumingii and Cristaria plicata live in fresh water,collectively known as freshwater pearl stratum powder.Pteria martensii live in sea water,so it is called seawater pearl stratum powder.Pearl stratum powder has the functions of calming the liver,calming astonishment,clearing heat and stopping bleeding.In clinic,it is mostly used to treat gastric and duodenal ulcer,neurasthenia,dizziness,tinnitus,palpitation,insomnia,sore throat,madness,epilepsy,etc.According to the literature,the main components of pearl stratum powder are protein and other organic components,calcium carbonate,trace elements and other inorganic components.17 kinds of amino acids can be obtained after protein hydrolysis.Each of these components plays an important role in the pharmacodynamics of pearl stratum powder.Each component plays an important role in the pharmacodynamics of pearl stratum powder.But at present,the research on pearl stratum powder mainly focuses on the preparation method of pearl stratum powder,the application of pearl stratum powder as a natural biological material in inducing osteogenesis,the clinical application of pearl stratum powder as a traditional Chinese medicine in compound prescription,and the identification method of pearl stratum powder and pearl powder.Few studies have been done on the quality control of pearl stratum powder.At present,pearl stratum powder has not been listed in Ch.P..But as a kind of traditional Chinese medicine,pearl stratum powder is more and more widely used.It is particularly important to establish a comprehensive and reliable quality control method for pearl stratum powder.In this paper,the quality control method of pearl stratum powder was established from the point of view of the study of organic and inorganic components in pearl stratum powder.This method can provide some references for the study of quality standards of pearl stratum powder.Method:(1)Quality control of pearl stratum powder was carried out from the point of view of organic composition research,including the establishment of fingerprints of amino acids and the determination of amino acid content in pearl stratum powder by pre-column derivatization with high performance liquid chromatography and the determination of protein content in pearl stratum powder by Kj eldahl method.(2)Quality control of pearl stratum powder was carried out from the point of view of inorganic composition research,including establishment of XRD fingerprint,infrared spectrum,thermogravimetric analysis,scanning electron microscopy,determination of calcium carbonate content in pearl stratum powder,evaluation methods of pearl stratum powder in Songling Xuemaikang,etc.(3)Establishment of limit standards for pearl stratum powder,including establishment of limit standards for pesticide residues and heavy metals and determination of trace elements in pearl stratum powder.(4)Conventional examination items of Ch.P.(2015 edition,Part IV)and Guidance on Analysis and Testing Technology of the Chinese Pharmacopoela(2017 edition),such as total ash and acid-insoluble ash,etc.(5)Study on the sedative effect of pearl stratum powder on mice by small animal autonomous activity instrument.(6)In this paper,the quality standard of pearl stratum powder in local medicinal materials standard was improved and supplemented.Results:(1)The fingerprint of amino acids in pearl stratum powder was established for the first time.23 common peaks were obtained and 15 of them were identified.The results of similarity evaluation,cluster analysis and principal component analysis were highly consistent.It was inferred that the contents of aspartic acid,arginine,alanine,cystine and leucine in seawater pearl stratum powder should be higher than those in freshwater pearl stratum powder by principal component ordination map.The content of serine,threonine and phenylalanine in seawater pearl stratum powder should be lower than that in freshwater pearl stratum powder.The correctness of the conjecture was confirmed by the determination of amino acid content in pearl stratum powder.This method distinguished pearl stratum powder of two different sources:Hyriopsis cumingii and Pyrola martensii.The content of protein in pearl stratum powder was determined by Kjeldahl method.It was found that the content of protein in pearl stratum powder of seawater was higher than that in fresh water.(2)The XRD fingerprint of pearl stratum powder was established for the first time.Through the establishment of XRD fingerprint,combined with the identification of characters,similarity evaluation,cluster analysis and principal component analysis,the quality difference of pearl stratum powder was accurately identified according to the difference of topographic isomerism of different quality pearl stratum powder.The aragonite structure of pearl powder was observed by scanning electron microscopy and the content of calcium carbonate in pearl stratum powder was estimated.Thermogravimetric analysis showed the track of pearl stratum powder changing with temperature,and calculated the content of organic matter and calcium carbonate in pearl stratum powder.Fourier transform infrared spectroscopy(FTIR)was used to observe the abnormal infrared spectroscopy characteristics of biogenic aragonite,which was different from other calcium carbonate medicinal materials,and it could distinguish pearl stratum powder from other aragonite medicinal materials.Calcium red indicator titration method was used to determine the content of pearl stratum powder in compound prescription.Calcium red indicator titration method was used to determine the content of pearl stratum powder in compound(Songling Xuemaikang)and it could be used for the quality control of pearl stratum powder in compound.(3)The contents of 29 trace elements were determined by ICP-MS.The heavy metal limit standard of pearl stratum powder was established for the first time.Pesticide residues in pearl stratum powder were not detected by GC-MS and QuEChERS.(4)The content of acid-insoluble ash in pearl stratum powder was determined according to the requirement of Ch.P.(2015 edition,Part IV)and Guidance on Analysis and Testing Technology of the Chinese Pharmacopoela(2017 edition),The results showed that the content of acid-insoluble ash in all batches of pearl stratum powder was below 4%,which accorded with the requirements of the pharmacopoeia.(5)Pearl stratum powder had obvious sedative effects on mice observed by small animal autonomous activity instrument.(6)According to the existing projects under the Fujian Provincial Standard of Traditional Chinese Medicine and Sichuan Provincial Standard of Traditional Chinese Medicine,as well as the supplementary projects based on the experimental results of this study,the draft quality standard of pearl powder was preliminarily formulated.Conclusion:In this experiment,the quality control of pearl stratum powder was studied in terms of inorganic composition,organic composition,establishment of limit standards,determination of routine test items,evaluation of pharmacological effects and establishment of draft quality standards. |
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