| This dissertation was divided into four chapters.In Chapter 1, a detailed review was given to the resource chemistry of the medicinal plants in genus Salvia L. in China and resources utilization of solid wastes derived from the process of Salvia miltiorrhiza industrialition. Salvia miltiorrhiza Bge.(SM), is a member of the genus Salvia of Lamiaceae family, which is widely distributed in China, especially in Shandong, Shanxi, Anhui and Henan Province. Chemical and pharmacological researches have shown that SM contains various tanshinones, Salvianolic acids, polysaccharides, and so on. It has becoming a hotspot for its efficacies of anti-microbial, anti-inflammatory, antioxidant, anti-tumor, anti-platelet aggregation, anti-thrombotic, and so on. The medical and functional products of SM have been widely used in cardiovascular and cerebrovascular diseases. In this chapter, resource distribution, the utilization status of SM and resource utilization of wastes derived from the process of industrialization, and the utilization approach were reviewed, so as to provide reference and basis for the effective and comprehensive utilization of its resources.In Chapter 2, it was studied on the accumulation dynamic analysis of Salvianolic acids on aerial parts of SM during different growing periods and different types chemical cpmpositions were carried out on the samples from different areas. Salvianolic acids, nucleosides and amino acids were analysed by the ultraperformance liquid chromatography coupled with a triple quadrupole mass detector. Polysaccharides were tested based on method of phenol-concentrated sulphuric. Through clear the value of aerial parts of SM, and discussing the strategy on the development and utilization, so as to provide reference and basis for the resource utilization of the non-medicinal parts of SM. The results were as follows.The UPLC-TQ/MS method was applied to study on dynamic changes of the aerial parts of Salvia miltiorrhiza during different growth periods based on the content of seven kinds of salvianolic acids, and determine the value of the aerial parts of SM. Results shows that the stems and leaves of SM were rich in salvianolic acids, but tanshinones were not detected in them. The highest content of salvianolic acids, besides salvianolic acid A in stem and leaf were in July or in August and gradually dropped off till the lowest in December. The content of salvianolic acids in flowers reach maximum during full-bloom stage. The dynamic change trend isn’t obvious before full-bloom stage, and its content sharply dropped when flowers began to fade. The aerial parts of S. miltiorrhiza were abundant in salvianolic acids, especially rosmarinic acid and salvianolic acid B, the content in luxuriant growth period were significantly higher than SM radix et rhizome, which showed that the aerial parts were the important resources to obtain the salvianolic acids.The analysis of polysaccharides were determined by the method of phenol-concentrated sulphuric. The results showed that the content of polysaccharides in different parts of SM were in significance difference. The order from high to low was roots, flower and stems and leaves. The difference between varies areas were huge, the samples from Shandong and Jiangsu were relatively higher. In flowers the difference of contents during initial flowering stage and full-bloom stage was not obvious, and it droped sharply when the flowers began to fade.The analysis of amino acids and nucleosides were performed on an Acquity UPLC BEH Amide (100 mm×2.1 mm,1.7μm) column. The mobile phase was composed of A (5 mM ammonium formate and ammonium acetate solution,0.2% formic acid) and B (Acetonitrile with 1 mM ammonium formate, ammonium acetate solution and 0.2% formic acid) with a gradient elution:1-3 min,10% A; 3-9 min,10%-18% A; 9-15 min,18%-20% A; 15-16 min,20%-46% A. The flow rate of the mobile phase was 0.4 mL/min, the column temperature was maintained at 35℃. The injection volume was 2 μL. It turns out that the content of different samples is abundant but unequal. Results shows that the amino acids and nucleosides were all riched in SM, stems and leaves of SM and inflorescences.In Chapter3, the fingerprinting and quality standard for the stems and leaves of SM were established. Meanwhile, the optimum drying method of the stems and leaves of SM was investigated based on quality evaluation.The UPLC method was applied to establish a analysis method of the fingerprint of the stems and leaves of SM. And the method was established with rapid analysis, high sensitivity, complete chemical fingerprint information, good peak separation and distinctive characteristics, which can be used for the quality control of the stems and leaves of SM. The UPLC fingerprints of the stems of leaves of SM were obtained with very good resolution under the established chromatographic system.15 peaks in the chromatograms were selected for the fingerprint identification and quality control of the stems of leaves of SM. The quality of ten batches of samples from different areas were assessed by comparing their chromatographic fingerprints with the reference fingerprints obtained at the same time, and the similarity was all above 0.88. The method established for fingerprint was sensitive and fast, which was suitable for the quality control of the stems and leaves of SM.The quality standards were established based on 10 batches of SM caulis et folium samples from nationwide. Transverse section and powder were used for analysis of microscopic characteristics. TLC was adopted to analyze the Salvianolic acids components. Total ash,and acid-insoluble ash were determined by methods in the appendices of Chinese Pharmacopoeia. The content of Salvianolic acids and flavonoids was determined by HPLC. Results:The characteristic of the organizational structure of the Salvia miltiorrhiza caulis et folium is obvious. The TLC was added and its spots developed were fairly and simply identical. The concentration of Salvianolic acids and flavonoids showed a good linear relationship at the linear range. Conclusion:The methods established in this paper such as microscopic identification, inspection, TLC identification and content determination were simple, sensitive and repeatable, which can be used for the quality standard of Salvia miltiorrhiza caulis et folium. The results of the research provide a scientific basis for the quality standard and utilization of Salvia miltiorrhiza caulis et folium.Five drying technology were compared in stems and leaves of SM including drying in sun or shade, hot air drying, infared drying, microwave drying and controlled temperature, in which fixing time and temperature were controlled. Suitable drying method was confirmed based on the color of dried samples and the content of Salvianolic acids and flavones. It was found that content of all compounds in fresh leaves, dried in sun or shade was lower than others. Finally,hot air drying at 50 ℃,60 ℃, and 60 ℃ after 60 s fixing at 100 ℃ was better than others which provided standards for drying supporting the quality of the stems and leaves of SM. Comprehensively considering of the shape of samples, drying efficiency and the contents of bioactive components, the hot-air drying after fixing and infrared drying at 50 ℃ temperature are the considerable drying method for the stems and leaves of SM.In Chapter 4, the optimum drying method of SM was investigated based on the mathematical model of moisture dynamics during the drying process of SM. And the dynamic change of resource chenmical composition during the drying process of SM was studied, so as to probe into the transformation mechanism of the bioactive components.The water dynamics model for drying process of SM was established based on the moisture ratio variation curves, the drying rate and drying activation energy with the drying methods of air drying, infrared drying and microwave drying under different temperatures (40 ℃,50 ℃,60 ℃, 70 ℃). It is found that the Page model could well describe the drying curves, for the moisture ratio vs. drying time profiled of the model showed high correlation (R2=0.993～0.999), and the predicted value was consistent with the experimental value. The results proved that the drying process of SM belonged to falling-rate drying period, and water diffusion played a leading role in the drying process of SM. Therefore, the Page model can be used to predict the moisture removal of SM in the drying process, which is great significance for the drying process of prediction, control and process optimization. The results provide the technical basis for the use of modern drying technology for industrial drying of SM.An ultra-high performance liquid chromatography coupled with a triple quadrupole mass method has been established for the simultaneous determination of the 10 Salvianolic acids and 6 tanshinones in SM. An Acquity UPLC BEH C18 (100 mm× 2.1 mm,1.7μm) column was applied for all analysis. The mobile phase was composed of solvent A (0.1% of formic acid water) and solvent B (acetonitrile) with a gradient elution:0-6 min,3%～30% B; 6～7 min, 30%～40% B; 7～10 min,40%～95% B; 10～12 min,95% B; 12～12.2 min,95%～3% B. The flow rate of the mobile phase was 0.4 mL/min, and the column temperature was maintained at 35 ℃. The established method was applied to evaluating the effect of different drying methods on the quality of SM. The results showed that SM slices and whole roots dried in different methods kept the similar chemical compositions to that of fresh SM, while Salvianolic acids and tanshinones increased after dried compared with fresh SM. It was discovered that the temperature is closely related to the contents of Salvianolic acids, especially rosmarinic acid and Salvianolic acid B, which respectively reduced along with the temperature changing from 40 ℃ to 70 ℃. In addition, the differences of drying methods and pretreatment methods also have effect on the quality of SM, even if at the same temperature. Comprehensively considering of the shape of SM, drying efficiency and the contents of bioactive components, the hot-air drying and infrared drying at 60 ℃ temperature are the considerable drying method for SM.Meanwhile, samples were collected during the process of infrared drying at 50 ℃ every 3 or 5 hours, all tested analytes were determined to probe into dynamic change of the tested compounds during the drying process. The results showed that compared with the fresh sample, the contents of Salvianolic acids in SM increased in certain degree after dried, especially rosmarinic acid and Salvianolic acid B. Unlike Salvianolic acids, tanshinones exist in fresh SM in a certain amount, but the contents also increased after dried. Salvianolic acids and tanshinones are dehydration stress induced product during the post-harvest drying process.Through the above research on the resource chemistry and quality standard of stems and leaves of SM, demonstration of traditional non-medicinal parts of the value in use model, where research resources chemicals, using different methods to enhance their efficiency of resource use, and for the systematic analysis and evaluation development of effective non-medicinal parts provide a scientific basis, which is of great practical significance and long-term strategic significance for extending the industrial chain of SM. At the same time, it is helpful to promote green economic development of the Chinese medicine industry and generating social-economic-ecological benefits. |
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