基于聚乙二醇表面成膜法的青黛亲水性饮片制备及系统评价  

Preparation of hydrophilic Indigo Naturalis based on polyethylene glycol(PEG)surface film-forming method and evaluation

作　　者：张婷[1] 黄胜杰 邓璇 徐小蓉 贺亚男 冉飞 慈志敏[1] 杨明 韩丽[1] 张定堃[1] ZHANG Ting;HUANG Sheng-jie;DENG Xuan;XU Xiao-rong;HE Ya-nan;RAN Fei;CI Zhi-min;YANG Ming;HAN Li;ZHANG Ding-kun(State Key Laboratory of Southwestern Chinese Medicine Resources,Chengdu University of Traditional Chinese Medicine,Chengdu 611137,China;Key Laboratory of Modern Preparation of Chinese Materia Medica,Ministry of Education,Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China)

机构地区：[1]成都中医药大学西南特色中药资源国家重点实验室,四川成都611137 [2]江西中医药大学现代中药制剂教育部重点实验室,江西南昌330004

出　　处：《中国中药杂志》2021年第13期3213-3221,共9页China Journal of Chinese Materia Medica

基　　金：国家自然科学基金面上项目(81773918);四川省科技厅青年杰出科技人才项目(2019JDJQ0007);成都中医药大学杏林学者学科人才科研提升计划项目(CXTD2018006)。

摘　　要：采用聚乙二醇(polyethylene glycol,PEG)表面成膜法制备效果稳定的亲水性青黛饮片,探讨其最佳制备工艺,并对其微观性质、亲水性、解热药效及安全性进行系统评价。以平衡接触角为评价指标,采用单因素试验考察改性剂种类、改性剂用量、分散剂用量以及共研磨时间对青黛亲水性的影响。结果表明最优工艺为取固定用量PEG6000(6%)超声溶解于10%无水乙醇溶液,溶解后与青黛共置于研磨机中研磨2 min,取出后平铺于方盘,置60℃烘箱中干燥去除乙醇,即得PEG改性后的亲水性青黛饮片。在此条件下,扫描电子显微镜(scanning electron microscope,SEM)提示改性青黛的表面较普通青黛更为平整,能谱仪显示改性青黛氮(N)、钙(Ca)和硅(Si)元素的分布数量少于普通青黛。改性青黛的平衡接触角较改性前降低18.96°,极性分量与表面自由能增加22.222 m J·m^(-2),非极性分量降低7.277 m J·m^(-2)。采用多重光散射技术进一步评价水中分散性,结果显示普通青黛的透射率约为85%,而改性青黛的透射率约为75%,表明改性青黛在水中的分散性较普通青黛更好;青黛在水中的混悬率实验表明,回流1 h后,普通青黛有57%未润湿,而改性青黛全部润湿并分散进入水中;溶出度实验表明改性青黛的靛蓝与靛玉红溶出量有所增加,且溶出更稳定均匀。将大鼠随机分成空白组、模型组、阳性对照(乙酰氨基酚)组、普通青黛组、亲水性青黛组。给药后观察大鼠体温变化,测血清中的IL-1β、TNF-α含量和下丘脑组织中IL-1β、PGE_(2)含量。结果显示,普通青黛组和亲水性青黛组大鼠给药后,体温较模型组均明显下降,同时亲水性青黛组大鼠的IL-1β浓度降低(P<0.05)。说明青黛改性前后均具解热疗效,且改性后的青黛疗效更佳。对改性青黛进行急性毒性实验和最大给药量实验,发现小鼠无中毒现象。该研究创新性地以聚乙二醇为改性剂制Polyethylene glycol(PEG)surface film-forming method was used to prepare hydrophilic Indigo Naturalis decoction pieces with stable effect.The preparation process of modified Indigo Naturalis was optimized and its microscopic properties,hydrophilicity,antipyretic efficacy,and safety were systematically evaluated.With equilibrium contact angle as assessment index,the influence of modifier type,modifier dosage,dispersant dosage,and co-grinding time on water solubility of Indigo Naturalis was investigated by single factor test.The results showed that the optimal preparation process was as follows.The 6% PEG6000 is dissolved in 10% anhydrous ethanol solution by sonification and then the mixture is ground with Indigo Naturalis for 2 min.The resultant product is dried on a square tray in an oven at 60℃ to remove ethanol and thereby the PEG-modified hydrophilic Indigo Naturalis decoction pieces are yielded.The morphological observation under scanning electron microscope(SEM)indicated that the modified Indigo Naturalis had smoother surface than Indigo Naturalis,and energy spectrometer measurement showed that the nitrogen(N),calcium(Ca),oxygen(O),and silicon(Si)on the surface of modified Indigo Naturalis powder were less than those of Indigo Naturalis powder.Modified Indigo Naturalis had the equilibrium contact angle 18.96°smaller,polar component 22.222 m J·m^(-2)more,and nonpolar component 7.277 m J·m^(-2)smaller than the Indigo Naturalis powder.Multiple light scattering technique was employed to evaluate the dispersion in water and the result demonstrated that the transmittance of Indigo Naturalis and modified Indigo Naturalis was about 85% and 75%,respectively,suggesting the higher dispersity of modified Indigo Naturalis.The suspension rate of modified Indigo Naturalis in water was determined by reflux treatment.The result showed that 57% of Indigo Naturalis was not wetted after refluxing for1 h,while the modified Indigo Naturalis was all wetted and dispersed into water.The dissolution of indigo and indirubin of mod

关 键 词：青黛 亲水性 粉体改性 聚乙二醇 表面成膜法 

分 类 号：R283.6[医药卫生—中药学]