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正交设计优化双斛胶囊的总多糖水提取工艺
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| 篇名： | 正交设计优化双斛胶囊的总多糖水提取工艺 |
| TITLE： | |
| 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；根据单因素试验考察结果，采用L9（34）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。 |
| 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（34） orthogonal test was used to optimize 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. |
| 期刊： | 2019年第30卷第18期 |
| 作者： | 单冰冰，陈宽，李婷，田富月，张建永 |
| AUTHORS： | SHAN Bingbing，CHEN Kuan，LI Ting，TIAN Fuyue，ZHANG Jianyong |
| 关键字： | 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 |
| KEYWORDS： | Shuanghu capsules； Dendrobium nobile； Dendrobium officinale； Total polysaccharide； Phenol-sulphuric acid method； Content determination； Yield of extract； Orthogonal test； Technology optimization |
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