[关键词]
[摘要]
目的 以黄芩Scutellariae Radix(SR)、黄连Coptidis Rhizoma(CR)的提取物浸膏粉为研究对象,考察不同干燥方式及辅料对其吸湿性的影响。方法 采用常压干燥(conventional drying,CD)、真空干燥(vacuum drying,VD)和喷雾干燥(spray drying,SD)方式制备常用中药黄芩及黄连的提取物浸膏粉,以含水量、吸湿率、比表面积、中值径、粒径分布宽度、粒径范围、豪斯纳比、休止角、松密度、振实密度、间隙率、卡尔指数总计12个二级指标建立提取物浸膏粉的物理指纹图谱,将所得二级指标转换成均一性、堆积性、可压性、流动性和稳定性5个一级指标,进而筛选出最佳的干燥工艺;并对各物理参数进行主成分分析(principal component analysis,PCA)以及偏最小二乘分析(partial least squares analysis,PLS),分析各物理参数与吸湿行为的相关性;优选糊精、β-环糊精、预胶化性淀粉、无水乳糖、微晶纤维素5种辅料对吸湿性的影响,绘制出粉体的吸湿率-时间动态曲线,并推导出半平衡吸湿时间(t1/2)及平衡吸湿率(F∞)构成二维评价指标,评价其动态吸湿行为,筛选出最佳防潮辅料。结果 通过物理指纹图相似度研究得出:黄芩:喷雾干燥浸膏粉(SR-SD)相似度最佳为0.98、0.99、0.99,真空干燥浸膏粉(SR-VD)相似度为0.87、0.92、0.89,均优于常压干燥,真空干燥、喷雾干燥与常压干燥的相似度分别是0.95、0.69;黄连:3种干燥方式自身差异不大,喷雾干燥浸膏粉(CR-SD)相似度最佳为0.99、1.00、0.99,真空干燥、喷雾干燥与常压干燥的相似度分别是0.94、0.61。根据5个一级指标结果综合评价可以得出黄芩真空干燥方式较好,黄连喷雾干燥方式较好。通过矩阵热点图及PCA、PLS,对吸湿率影响最为显著的是粒径分布宽度、粒径范围、比表面积、中值径,其次为振实密度、松密度(P<0.05)。通过动态二维表征技术,得出辅料可以改善浸膏粉的吸湿性。研究表明:黄芩:浸膏粉的3种干燥方式下样品均属于第2类,平衡吸湿量大,吸湿速率慢,药辅混合物大部分属于第3类,平衡吸湿量小,吸湿速率慢,黄芩常压干燥样品与β-环糊精的药辅混合物平衡吸湿量最小,其值F∞=9.12%,黄芩真空干燥样品与β-环糊精的药辅混合物吸湿速率最小t1/2=69.33 h;黄连:常压和喷雾浸膏粉属于第2类,其药辅混合物均属于第3类,其中黄连真空样品与乳糖的药辅混合物,平衡吸湿量最小,其F∞=7.72%,黄连真空样品与β-环糊精的药辅混合物的吸湿速率最小,t1/2=76.33 h。结论 改善中药提取物的干燥方式,选取优质防潮辅料可以改善中药提取物的吸湿性。
[Key word]
[Abstract]
Objective Taking Huangqin (Scutellariae Radix, SR) and Huanglian (Coptidis Rhizoma, CR) extract powder as the research object, the effects of different drying methods and auxiliary materials on moisture absorption were investigated. Methods The extract powder of SR and CR were prepared by conventional drying (CD), vacuum drying (VD) and spray drying (SD). Twelve secondary indexes, such as moisture content, moisture absorption rate, specific surface area, median diameter, span, width, Hausner ratio, angle of repose, bulk density, tapped density, gap rate, and Carr index, were used to establish the physical fingerprint of extract powder. The secondary indexes were converted into five primary indexes including uniformity, pileup, compressibility, fluidity and stability. Then the best drying process was selected. Principal component analysis (PCA) and partial least squares analysis (PLS) were used to analyze the correlation between the physical parameters and the moisture absorption behavior. The effects of five excipients, including dextrin, β-cyclodextrin, pre-gelatinized starch, anhydrous lactose and microcrystalline cellulose, on the moisture sorption of the powder were optimized. The dynamic curve of moisture sorption time of the powder was drawn, and the semi-equilibrium moisture sorption-time (t1/2) and equilibrium moisture sorptiontime (F∞) were derived to form a two-dimensional evaluation index to evaluate the dynamic moisture sorption behavior of the powder and screen out the best moisture-proof excipients. Results Based on the physical fingerprint similarity study, the following results were obtained:SR:The best similarity of spray drying extract powder (SR-SD) was 0.98, 0.99, 0.99, and the similarity of vacuum drying extract powder (SR-VD) was 0.87, 0.92, 0.89, which was better than that of atmospheric pressure drying. The similarity of vacuum drying, spray drying and atmospheric pressure drying was 0.95, 0.69, respectively. CR:There was no significant difference among the three drying methods. The best similarity of spray drying extract powder (CR-SD) was 0.99, 1.00 and 0.99, and the similarity of vacuum drying, spray drying and atmospheric pressure drying were 0.94 and 0.61, respectively. According to the comprehensive evaluation of 5 first-level indicators, it can be concluded that the vacuum drying mode and the spray drying mode are better. Through the matrix heat map, PCA and PLS, span, width, SSA and D50 had the most significant influence on H, followed by Dc and Da (P < 0.05). Through dynamic two-dimensional characterization technology, it can be observed that the excipients can improve the moisture absorption of the powder. The research shows that:SR:Under the three drying methods of extract powder, the samples belong to the second class, with large equilibrium moisture absorption capacity and slow moisture absorption rate, and the medication-auxiliary mixture belongs to the third class, with small equilibrium moisture absorption capacity and slow moisture absorption rate. Among them, the equilibrium moisture absorption of the atmospheric dried sample of SR and the medication-auxiliary mixture of β-cyclodexmin is the smallest, with F∞=9.12%. Vacuum-dried samples of SR and the drug-adjuvant mixture of β-cyclodextrin had the lowest moisture absorption rate, t1/2=69.33 h, CR:The atmospheric pressure and spray extract powder belong to the second class, and the drug-auxiliary mixture belongs to the third class. The equilibrium moisture absorption of the drug-auxiliary mixture of CR vacuum sample and lactose is the smallest, with F∞=7.72%, and the moisture absorption rate of the drug-auxiliary mixture of CR vacuum sample and β-cyclodextrin is the smallest, t1/2=76.33 h. Conclusion Improving the drying method of traditional Chinese medicine extracts and selecting high-quality moisture-proof excipients can improve the moisture absorption of Chinese medicine extracts.
[中图分类号]
R283.6
[基金项目]
江苏省“青蓝工程”中青年学术带头人资助项目(2021年);江苏省“青蓝工程”优秀青年骨干教师资助项目(2021年);江苏省高校自然科学基金(21KJB360021);江苏省高校自然科学基金(22KJB360014);泰州市社会发展支撑项目(SSF20220004);江苏省中医药科技发展计划项目(YB2020108);江苏省大学生创新创业训练计划项目(202313981009Y)