基于《雷公炮炙论》的白矾蜂巢制炮制工艺研究

Research on preparation technology of wax Alumen based on Lei’s Treatise on Preparing Drugs

目的传承古法,建立白矾蜂巢制的炮制工艺。方法以炮制品外观性状、硫酸铝钾的含量、蜂巢制白矾粉末色度、溃疡损伤程度为指标,采用单因素结合星点设计-响应面法对白矾蜂巢制炮制工艺进行考察。最后采用扫描电镜法和红外光谱法对白矾、蜂巢制白矾及煅制品枯矾进行鉴别与质量控制。结果确定了白矾蜂巢制的最佳炮制工艺为取白矾样品,置于煅药炉中煅烧,加热温度为(587±5)℃,加热时间为60 min,取出,趁热加入0.6倍量蜂巢,保持温度继续加热180 min,取出晾凉后,研成粉末状,用麻纸包裹,埋于深12~15 cm的土壤中,土壤温度为20~25℃,土壤水分为20%~40%,坑埋时长为12 h,即得。白矾炮制前后微观形态变化显著,炮制品粒子粒度变小,表面结构更粗糙,疏松多孔结构明显,蜂巢制白矾与煅制品枯矾相比表面的碎屑呈圆柱状或椭圆状,加入蜂巢使晶体结构出现融合现象,晶体边缘更加圆钝。白矾的红外光谱特征峰为618、918、1113、1670、3441 cm^(−1),蜂巢制白矾的特征峰为472、617、688、1121、1242、1640、3446 cm^(−1),枯矾的特征峰为477、618、688、1112、1645、3458 cm^(−1),3者峰形和峰强度存在明显差异,且相似度分析和聚类分析结果均显示3者具有显著性差异。结论白矾蜂巢制工艺遵古继承了《雷公炮炙论》中的传统炮制方法,保留了传统煅制的特点,量化了关键操作技术点温度以及前后时间等重要参数,经验证工艺条件稳定、合理、可行性强,为大工业的生产提供了理论基础。扫描电镜和红外光谱分析法可以从微观形态层面和成分结构变化2个方面对白矾生品、蜂巢制白矾和枯矾进行鉴别与质量控制。

Objective To inherit the ancient method and establish the preparation technology of wax Baifan(Alumen).Methods Using the appearance of the artifacts,the content of potassium aluminum sulfate,the color of alum powder from honeycomb,and the degree of ulcer damage as the indicators,a one-way combination of star point design and response surface methodology was used to investigate the artifacts of alum from honeycomb.Finally,electron microscope scanning and infrared spectroscopy were used for the identification and quality control of alum,honeycomb alum and calcined alum.Results Determined the optimal concoction process of alum honeycomb system for alum samples,placed in the calcining furnace calcination,heating temperature of(587±5)℃,heating time of 60 min,remove,add 0.6 times the amount of honeycomb while hot,keep the temperature continue to heat for 180 min,remove to cool,research into powder,wrapped in linen paper,buried in a depth of 12—15 cm in the soil,the soil temperature 20—25℃,soil moisture of 20%—40%,the length of 12 h that is obtained.Soil temperature was 20—25℃,soil moisture was 20%—40%,and the length of pit burial was 12 h,which was obtained.The microstructure of alum changed significantly before and after the preparation,the particle size of the product became smaller,the surface structure was rougher,and the loose porous structure was obvious,and the debris on the surface of the honeycomb alum compared with the calcined alum was cylindrical or elliptical,and the addition of honeycomb made the crystal structure fusion,and the edges of the crystals were more round and blunt.The characteristic peaks of the infrared spectrum of alum were 618,918,1113,1670,3441 cm^(−1),and the characteristic peaks of honeycomb alum were 472,617,688,1121,1242,1640,3446 cm^(−1),and those of chrysotile were 477,617,688,1121,1242,1640,3446 cm^(−1),and those of calcined alum The peaks were 477,618,688,1112,1645,3458 cm^(−1),and the peak shapes and peak intensities of the three peaks were obviously different,and the results of similarity analysis and cluster analysis showed that the three peaks were significantly different.Conclusion The process of alum honeycomb system inherited the traditional concoction method in Lei’s Treatise on Preparing Drugs in accordance with ancient times,retained the characteristics of traditional calcination,quantified the important parameters such as the temperature of the key operation technology point and the time before and after,and verified that the process conditions were stable,reasonable and feasible,which provided a theoretical basis for the production of large-scale industry.Electron microscope scanning and infrared spectroscopy analysis can be used to identify and quality control raw alum,honeycomb-made concoctions and withered alum from both the micro-morphological level and the compositional and structural changes.