Page 65 - 2019年9月第30卷第18期
P. 65
正交设计优化双斛胶囊的总多糖水提取工艺 Δ
#
*
单冰冰 ,陈 宽,李 婷,田富月,张建永(遵义医科大学药学院,贵州 遵义 563000)
中图分类号 R284.2;R943 文献标志码 A 文章编号 1001-0408(2019)18-2508-05
DOI 10.6039/j.issn.1001-0408.2019.18.11
摘 要 目的:优化双斛胶囊总多糖的水提取工艺。方法:对双斛胶囊组方药材金钗石斛和铁皮石斛混合物在以醇提取总生物碱
之后进行水提取总多糖。以葡萄糖为对照品,采用硫酸-苯酚法显色处理并在488 nm波长处检测,测定总多糖含量。以干膏得率
和总多糖含量计算的综合评分为评价指标,采用单因素试验考察料液比、提取温度、提取时间和提取次数对提取效果的影响;根据
4
单因素试验考察结果,采用L9 (3)正交表进行设计和试验,进一步优化料液比、提取温度、提取时间、提取次数等条件,并对所得优
化工艺进行验证试验。结果:葡萄糖质量浓度在0.041 4~0.207 0 mg/mL范围内与吸光度的线性关系良好(r=0.999 9);日内、日
间RSD为3.61%~8.24%(n=3、n=5),重复性试验RSD为1.49%(n=6);平均加样回收率为98.65%(RSD=1.45%,n=6)。优化
后的水提取工艺为料液比1∶25(g/mL)、提取温度100 ℃、提取时间90 min、提取1次;3次验证试验结果显示,优化工艺所得水提物
的平均总多糖含量为379.292 8 mg/g(RSD=1.93%,n=3)、平均干膏得率为22.75%(RSD=2.41%,n=3)。结论:所建立的硫酸-
苯酚法简便,精密度、准确度均良好;优化所得的水提取工艺稳定、可行,可用于双斛胶囊总多糖的提取。
关键词 双斛胶囊;金钗石斛;铁皮石斛;总多糖;硫酸-苯酚法;含量测定;干膏得率;正交试验;工艺优化
Optimization of Water Extraction Technology of Total Polysaccharide of Shuanghu Capsules by
Orthogonal Design
SHAN Bingbing,CHEN Kuan,LI Ting,TIAN Fuyue,ZHANG Jianyong(School of Pharmacy,Zunyi Medical
University,Guizhou Zunyi 563000,China)
ABSTRACT OBJECTIVE: To optimize the water extraction technology of total polysaccharide of Shuanghu capsules.
METHODS:The total alkaloid was firstly extracted from Dendrobium nobile and Dendrobium officinale mixture of Shuanghu
capsules with ethanol,and then total polysaccharide was extracted with water. Using glucose as control,total polysaccharide was
treated with phenol-sulfuric acid method and its content was determined at 488 nm. Using comprehensive score calculated with the
yield of the extract and the content of total polysaccharide as index,the effects of material-liquid ratio,extraction temperature,
extraction time and times on the extraction were investigated by single factor test. Then L9 (3)orthogonal test was used to optimize
4
solid-liquid ratio,extraction temperature,extraction time and extraction times according to the results of single factor test. The
optimized technology was validated. RESULTS:The linear range of glucose were 0.041 4-0.207 0 mg/mL(r=0.999 9). RSDs of
intra-day and inter-day ranged 3.61%-8.24%(n=3,n=5),and RSD of repeatability test was 1.49%(n=6). Average recovery
rate was 98.65%(RSD=1.45%,n=6). The optimal water extraction technology included solid-liquid ratio of 1 ∶ 25(g/mL),
extraction temperature of 100 ℃,extracting for 90 min,extracting once. Results of validation tests showed that average content of
total polysaccharide was 379.292 8 mg/g(RSD=1.93%,n=3)and average yield of the extract was 22.75%(RSD=2.41%,n=3).
CONCLUSIONS: Established phenol-sulphuric acid method is simple, precise and accurate. The optimal water extraction
technology is stable and feasible,which can be used for the extraction of total polysaccharides from Shuanghu capsules.
KEYWORDS Shuanghu capsules;Dendrobium nobile;Dendrobium officinale;Total polysaccharide;Phenol-sulphuric acid
method;Content determination;Yield of extract;Orthogonal test;Technology optimization
流行病学调查结果显示,我国饮酒人群比例和酒精 酒精性肝损伤(Alcoholic liver disease,ALD),ALD 贯穿
性肝病发病率均呈上升趋势,酒精性肝病已成为我国最 于酒精性肝病发生的始终 。但目前 ALD 的发病机制
[2]
主要的慢性肝病之一,其可导致机体多系统、多器官损 尚未阐明,西医治疗以戒酒、营养支持及对症治疗为主,
[1]
伤,危害不容小觑 。酒精性肝病最基本的病理状态是 尚缺乏特效药物 。中医辨证论治是中医理论的精华,
[3]
Δ 基金项目:贵州省科技计划项目(No.黔科合重大专项字[2015] 其认为ALD是由酒毒湿热之邪熏蒸肝胆,致痰浊凝聚、
6010-1);贵州省普通高等学校科技拔尖人才支持计划(No.黔教合KY 肝失调达、气血郁滞、脾胃损伤。虽然中医学者和医家
字[2017]078) 尚未对ALD的辨证进行统一,但治法多以清热化湿、理
*硕士。研究方向:中药新药研发。电话:0851-28642517。E-
气化瘀、补益肝肾为主 [4-6] 。因此,如能在辨证论治的指
mail:494814886@qq.com
导原则下,结合现代药理学研究成果,可更有针对性地
# 通信作者:副教授,硕士生导师,博士。研究方向:中药质量评
价。电话:0851-28642517。E-mail:zhangjianyong2006@126.com 选择药物,使患者获得更好的疗效。
·2508 · China Pharmacy 2019 Vol. 30 No. 18 中国药房 2019年第30卷第18期