| Mineral medicine is an important part of Chinese medicine,including natural rock minerals,paleontological fossils,as well as synthetic of rock minerals and clay minerals.China has a long history of applying mineral medicines.In the Spring and Autumn Period and the Warring States period,the Shan Hai Jing recorded four kinds of mineral medicines,including cinnabar and arsenic.Six kinds of mineral medicines were recorded in the Wanwu from Fuyang Bamboo Slips.21 species of mineral medicines were recorded in the recipes for Fifty-two atlments.46 kinds of mineral medicines were collected in the Shen Nong's classic of Materia Medica in the Eastern Han Dynasty.161 species of mineral medicines were included in the Compendium of Materia Medica in the Ming Dynasty,and 38 species were added to the Supplement to the Compendium of Materia Medica.82 kinds of mineral medicines were collected in Chinese medicine dictionary(1985 edition),which is a modern Chinese medicine book.At present,122 kinds of mineral medicines are collected at domestic pharmaceutical standards at all levels,among which 24 are included in the Chinese Pharmacopoeia(2015 edition).About 7% of the prescriptions of proprietary Chinese medicines contain mineral medicines;mineral medicines for modern clinical use are 50~60 species.However,the simple description of mineral medicines in Materia Medica leads to the widespread phenomenon of synonyms and homonyms.On the one hand,there are often harmful elements in mineral medicines.On the other hand,mineral medicines in different areas are effected by geological processes,which causes their components are complex and not identical.Therefore,the quality control of mineral medicines has received widespread attention.In this study,we chose the commonly used 16 kinds of mineral drugs as the research object.X-ray fluorescence spectroscopy(XRF)analysis technology were used to analyze the elements in mineral drugs from oxygen to uranium to explore a rapid detection method for identification and quality control of mineral medicines.The main results are as follows:(1)The situation of commercially available products of 16 mineral medicines was clarified.Among the 153 samples of mineral medicines collected from major pharmaceutical companies,69 samples(45.1%)were identified with trait identification characteristics,and 84 samples(54.9%)were powders or granules.Trait identification results showed that there are less adulteration in Gypsum,Pyritum,Spirifer and Talcum,and there are more adulteration Fluoritum,Ophicalcitum,Os Draconis and Dens Draconis,followed by Stalactitum and Chloriti Lapis.At the same time,the proportion of powdered or granular products is relatively large,which also puts new requirements on the identification and quality control of mineral medicines.(2)The XRF analysis method for mineral medicines was optimized and its application scope was clarified.Through the optimization of the X-ray fluorescence spectrum conditions,69 elements in the sample were detected at one time.By comparing the method of pressed powder pellet,all samples were divided into three categories:(1)The sample with good adhesion was directly compressed by the plastic ring pressing method;(2)The samples with poor adhesion were taken with boric acid trim.,Bottom,tablet;(3)The samples with very poor adhesiveness of the sample,add appropriate amount of adhesive(such as microcrystalline cellulose)fully mixed,set around and bottom with boric acid,and then pressed it.The gypsum(GBW03111a)and fluorite(GBW07252)standard samples were tested according to the proposed method in this study.The relative error between the test values and the standard value of the identified elements in the prototype certificate was 0.01 to 13.15%.It also shows that the XRF analysis method has a large error for the identification of elements below 5 ppm,and it cannot be used for mineral medicine rich in crystal water,such as Glauber's salt and alum.(3)XRF fingerprinting analysis method for mineral medicine(without crystal water)and XRF fingerprinting of 16 common mineral medicines were established.To directly show the X-ray fluorescence spectrum of mineral medicine,a plot of the square root of K,L,M line intensity and 2? angle is made,and then marked the information of elements,set up of fingerprint of minerals medicine XRF.The method can distinguish calcium mineral medicine,iron mineral medicine,silicon mineral medicine,aluminum mineral medicine,and sodium mineral medicine,For example,it can effectively distinguish hard talc and soft talc powder samples,However,this method still needs to be optimized,due to the limitations in the identification of genuine,fake and adulterated products.(4)22 quantitative working curves were established for the analysis of mineral drug elements.70 national standards for standard substances similar to common mineral medicines,including rock samples,standard sediment samples and soil samples,were used to establish 22 quantitative working curves for mineral element analysis.Through the methodological inspection of precision and accuracy,it can meet the analysis requirements,and provide experimental basis for further establishing a rapid identification and quality control method that is suitable for a large number of mineral medicine.In summary,the proportion of powdered or granular commercial products of commercial mineral medicines is relatively large,which puts forward new requirements for the identification and quality control of mineral medicines.In this study,by optimizing the analysis conditions of XRF,based on the analysis of 16 mineral drugs,a preliminary XRF fingerprinting analysis method for mineral drugs(without crystal water)were established and 22 quantitative working curves were measured.It has enriched the identification methods of mineral medicines,and laid the foundation for the rapid identification of mineral medicines and quality control method.This study has important significance for the identification of mineral medicine powders. |
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