抗瘤增效方浓缩工艺研究  

Research on concentration process of Kangliu Zengxiao Formula

作　　者：吴阳阳 赵春草[1] 李更青 赵晓珍[2] 吴飞[1] 张继全[1] WU Yangyang;ZHAO Chuncao;LI Gengqing;ZHAO Xiaozhen;WU Fei;ZHANG Jiquan(Engineering Research Center of Modern Preparation Technology of TCM,Ministry of Education,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Department of Oncology,Longhua Hospital Affiliated lo Shanghai University of Traditional Chinese Medicine,Shanghai 200032,China)

机构地区：[1]上海中医药大学中药现代制剂技术教育部工程研究中心,上海201203 [2]上海中医药大学附属龙华医院肿瘤科,上海200032

出　　处：《上海中医药大学学报》2020年第3期76-82,共7页Academic Journal of Shanghai University of Traditional Chinese Medicine

基　　金：上海市进一步加快中医药事业发展三年行动计划中医医院制剂能力提升项目(ZY3-JSFC-2-2006);上海市科委科技支撑项目(17401902600)。

摘　　要：目的:研究抗瘤增效方中指标性成分毛蕊异黄酮葡萄糖苷和盐酸小檗碱在浓缩过程中的热稳定性,制定浓缩工艺参数,并以特征图谱法进行验证。方法:建立高效液相色谱(HPLC)法检测抗瘤增效方中毛蕊异黄酮葡萄糖苷和盐酸小檗碱的含量。在60~90℃范围内,考察常压和减压浓缩状态下抗瘤增效方的热稳定性规律,以确定提取液的浓缩工艺参数,并建立HPLC特征图谱对浓缩工艺进行进一步验证。结果:在60~90℃范围内,常压或减压浓缩8 h过程中,毛蕊异黄酮葡萄糖苷和盐酸小檗碱的转移率保持稳定。结合生产实践,初步确定抗瘤增效方的浓缩工艺为70℃减压浓缩。所建立的HPLC特征图谱含有10个共有峰(包含毛蕊异黄酮葡萄糖苷和盐酸小檗碱),特征图谱相似度>0.93,峰面积变化率<20%。结论:抗瘤增效方浓缩过程中毛蕊异黄酮葡萄糖苷和盐酸小檗碱均无明显的热敏性,70℃减压浓缩的工艺条件合理、可行。Objective: To study the thermal stability of the two index components calycosin-7-glycoside and berberine hydrochloride in Kangliu Zengxiao Formula during the concentration process and determine the concentration process parameters, which verified by characteristic chromatogram. Methods:A high performance liquid chromatography(HPLC) method was established for the content determination of calycosin-7-glycoside and berberine hydrochloride in Kangliu Zengxiao Formula. In the range of 60-90 ℃, the thermal stability of Kangliu Zengxiao Formula was observed under the atmospheric pressure and decompression concentration, so as to determine the concentration process parameters of the extract. The HPLC characteristic chromatogram was established to further verify the concentration process.Results: In the range of 60-90 ℃, during 8 hours of atmospheric pressure or decompression concentration, the transfer rates of calycosin-7-glycoside and berberine hydrochloride both maintained stable. Combined with the production practice, the concentration process of Kangliu Zengxiao Formula was preliminarily determined to be decompression concentration at 70 ℃.There were 10 common peaks marked in HPLC characteristic chromatogram, including calycosin-7-glycoside and berberine hydrochloride. The similarity of characteristic chromatogram was more than 0.93, and the change rate of peak area was less than 20%.Conclusion: Neither calycosin-7-glycoside nor berberine hydrochloride in Kangliu Zengxiao Formula show obvious heat sensitivity during the concentration process.The process conditions of decompression concentration at 70 ℃ are reasonable and feasible.

关 键 词：抗瘤增效方 浓缩工艺 热稳定性 毛蕊异黄酮葡萄糖苷 盐酸小檗碱 高效液相色谱法 特征图谱 

分 类 号：TQ461[化学工程—制药化工]