[关键词]
[摘要]
目的 采用表面改性技术优化黄芩(Scutellariae Radix,SR)、黄连(Coptidis Rhizoma,CR)浸膏粉的综合性能,优选最佳改性剂及改性工艺,为后续制剂开发提供依据。方法 制备黄芩、黄连浸膏粉及流浸膏,选择二氧化硅(silicon dioxide,S)、微粉硅胶(micronized silica gel,M)、羟丙基甲基纤维素(hydroxypropyl methylcellulose,H)3种改性剂,采用表面包覆(surface cladding,SC)和微囊化包衣(microencapsulation coating,MC)2种改性技术分别制备改性浸膏粉。测定各浸膏粉的吸湿率(H)、含水量(HR)、休止角(α)、松密度(Da)、振实密度(Dc)、豪斯纳比(IH)、卡尔指数(IC)、间隙率(Ie)、中值径(D50)、粒径分布宽度(span)、粒径范围(width)及比表面积(SSA)总计12个二级指标,进行归一化处理,绘制物理指纹图谱并进行相似度分析。将二级指标转换成均一性、堆积性、流动性、可压性和稳定性共5个一级指标,采用熵权-变异系数法获得权重系数,并计算各浸膏粉综合性能评分。选用主成分分析法(principal component analysis,PCA)评价各二级指标对浸膏粉综合性能的贡献率,针对影响浸膏粉均一性最为显著的D50进行偏最小二乘法(partial least squares,PLS)分析,明确各二级指标与其相关性。结果 SC和MC改性技术,制备获得SR、CR浸膏粉及6种改性浸膏粉,各浸膏粉二级指标归一化处理,绘制物理指纹图谱。相似度研究得出:黄芩SR与SC改性组SR-SC-S、SR-SC-M、SR-SC-H的相似度分别为0.977、0.971、0.978;SR与囊化包衣改性组SR-MC-S、SR-MC-M、SR-MC-H的相似度分别为0.717、0.739和0.693。黄连CR与SC改性组CR-SC-S、CR-SC-M、CR-SC-H的相似度分别为0.904、0.902和0.955,CR与囊化包衣改性组CR-MC-S、CR-MC-M、CR-MC-H浸膏粉的相似度分别为0.729、0.737和0.716。MC改性的SR、CR与未改性浸膏粉相比具有显著性差异,羟丙甲基纤维素改性剂差异最显著,SC改性工艺改性组效果不明显,无显著性差异。熵权变异系数法计算得出,黄芩耦合权重系数wjSR:稳定性(0.121 0)、均一性(0.484 0)、流动性(0.186 7)、堆积性(0.099 0)、可压性(0.109 3);黄连耦合权重系数wjCR:稳定性(0.013 4)、均一性(0.394 1)、流动性(0.173 1)、堆积性(0.288 5)、可压性(0.130 9)。浸膏粉性能综合性能评分结果显示,黄芩SR浸膏粉综合性能评分49.13,MC改性SR-MC-H、SR-MC-M、SR-MC-S综合性能评分分别为62.90、61.78、61.64,相比具显著差异,SR-MC-H综合性能评分较浸膏粉提高了28.0%,改性最佳,SC改性效果略差。黄连CR浸膏粉综合性能评分为50.21,MC改性综合性能评分均大于61.00,与浸膏粉相比差异具有显著性,CR-MC-H综合性能评分61.68,较未改性组提高了22.8%,效果最佳,SC改性,二氧化硅及微粉硅胶组浸膏粉综合性能评分分别为56.35、56.25,也有显著性差异。PCA结果表明α、SSA、HR、width、span这5个二级指标对SR、CR浸膏粉综合性能贡献率较大。针对D50进行PLS分析,得出width、span、H及Dc等指标对浸膏粉D50影响较为显著。结论 表面改性技术可提高黄芩、黄连浸膏粉的综合性能,MC改性工艺改性效果较好,羟丙基甲基纤维素作为改性剂综合性能评分最高。
[Key word]
[Abstract]
Objective Surface modification technology was used to optimize the comprehensive properties of Scutellariae Radix (SR) and Coptidis Rhizoma (CR) extract powders. The study aimed to select the best modifier and process, providing a foundation for the development of subsequent formulations. Methods SR and CR extract powders and crude extracts were prepared. Three modifiers , silicon dioxide (S), micronized silica gel (M) and hydroxypropyl methylcellulose (H), were selected, and the modified technology of surface cladding (SC) and microencapsulation coating (MC) was used to prepare modified extract powder. Powders were measured secondary indexes, including H, HR, α, Da, Dc, IH, IC, Ie, D50, span, width and SSA. All secondary indexes were normalized and a physical fingerprint diagram was drawn and similarity analysis was conducted. The secondary indexes were converted into five primary indexes of uniformity, accumulability, flowability,compressibility and stability, and the weight coefficients were obtained by using the entropy weighted coefficient of variation method. The comprehensive performance scores of the extract powders were calculated. PCA was used to evaluate the contribution rate of each secondary index to the comprehensive performance of the extract powders, and PLS was used to analyze the correlation between each secondary index and the comprehensive performance of the extract powders, focusing on the D50 that the greatest impact on the homogeneity of the extract powders. Results Using SC and MC modification techniques, SR, CR, and six modified extract powders were prepared. The secondary indexes of each extract powder were normalized, and physical fingerprint profiles were created. The similarity analysis results were as follows: The similarity between SR and SC modified groups SR-SC-S, SR-SC-M, and SR-SC-H was 0.977, 0.971, and 0.978, respectively. The similarity between SR and MC modified groups SR-MC-S, SR-MC-M, and SR-MC-H was 0.717, 0.739, and 0.693, respectively. The similarity between CR and SC modified groups CR-SC-S, CR-SC-M, and CR-SC-H was 0.904, 0.902, and 0.955, respectively. The similarity between CR and MC modified groups CR-MC-S, CR-MC-M, and CR-MC-H was 0.729, 0.737, and 0.716, respectively. Significant differences were observed between the MC modified SR and CR powders compared to the unmodified extract powders, with hydroxypropyl methylcellulose showing the most significant difference. The SC modification showed no significant effect. The entropy weight coefficient of variation method yielded the following coupling weight coefficients wjSR: stability (0.121 0), uniformity (0.484 0), flowability (0.186 7), accumulability (0.099 0), and compressibility (0.109 3); wjCR: stability (0.013 4), uniformity (0.394 1), flowability (0.173 1), accumulability (0.288 5), and compressibility (0.130 9). The results of comprehensive performance scores of the extract powders showed the comprehensive performance score of SR extract powder was 49.13. The MC modified SR-MC-H, SR-MC-M, and SR-MC-S had comprehensive performance scores of 62.90, 61.78, and 61.64, respectively, showing significant differences compared to the unmodified powder. The SR-MC-H comprehensive performance score improved by 28.0% over the unmodified extract powder, indicating the best modification effect, while the effect of SC modification was slightly worse. The comprehensive performance score of CR extract powder was 50.21. The MC modified powders had comprehensive performance scores above 61.00, showing significant differences compared to the unmodified powder. The CR-MC-H had a comprehensive performance score of 61.68, an improvement of 22.8% over the unmodified group, indicating the best effect. The SC modification with silicon dioxide and micronized silica gel resulted in comprehensive performance scores of 56.35 and 56.25, respectively, also showing significant differences. PCA analysis indicated that five secondary indexes α, SSA, HR, width, and span had a large contribution to the overall performance of SR and CR extract powders. PLS analysis of D50 revealed that width, span, H, and Dc had significant effects on the D50 of the extract powders. Conclusion Surface modification technology can improve the comprehensive properties of SR and CR extract powders. The MC modification technology showed the best results, with hydroxypropyl methylcellulose achieving the highest comprehensive performance score as a modifier.
[中图分类号]
R283.6
[基金项目]
江苏省“青蓝工程”优秀教学团队资助项目(2024年);泰州市科技支撑计划(社会发展)项目(TS202425,SSF20230030);泰州职业技术学院科研课题(TZYKY-21-5);江苏省大学生创新创业训练计划项目(202413981004Y)