| 复方首乌藤合剂的总多糖含量测定及单糖组分分析 |
| 投稿时间：2019-08-06 修订日期：2019-12-11 点此下载全文 |
| 引用本文：叶财发,蔡跃辉,曾棋平,曹毅祥,陈锦珊.复方首乌藤合剂的总多糖含量测定及单糖组分分析[J].药学实践杂志,2020,38(2):161~165 |
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| 基金项目:医院青年苗圃课题（16Y024）；福建中医药大学临床专项校管课题（NO.XB2017080） |
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| 中文摘要:目的 建立复方首乌藤合剂总多糖含量测定方法，并分析多糖组分。方法 采用水提醇沉法提取复方首乌藤合剂多糖，经苯酚-硫酸法处理后，再利用紫外分光光度法测定该制剂中总多糖含量；另外，多糖经三氟乙酸水解后，用1-苯基-3-甲基-5-吡唑啉酮（PMP）衍生多糖水解产物，再利用高效液相色谱法，依利特krosmasil-C 18色谱柱 (4.6 mm×250 mm，5 μm)，柱温：30 ℃，以乙腈-0.1 mol/L磷酸盐缓冲液(pH=6.8)（18：82）为流动相，进行等度洗脱；流速：1.0 ml/min；检测波长250 nm，进样量：20 μl。分析4批次复方首乌藤合剂多糖中的单糖组分。结果 D-无水葡萄糖质量浓度在21~105 μg/ml范围内与吸光度线性关系良好，线性回归方程为Y= 0.007X + 0.010 5，r = 0.998 2；平均加样回收率为(100.45±1.57)% (n=6)；4 批样品测得的总多糖平均含量为14.24、21.09、17.85、18.17 mg/ml；复方首乌藤合剂多糖主要由甘露糖、盐酸氨基葡萄糖、半乳糖醛酸、葡萄糖、半乳糖、阿拉伯糖等6个单糖组成，各个单糖峰面积比约为9.10：0.26：1.00：3.02：4.14：2.12。结论 该方法准确、可靠，可用于该制剂中总多糖含量测定及单糖组分分析。 |
| 中文关键词:复方首乌藤合剂 总多糖 紫外分光光度法 单糖 高效液相色谱法 |
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| Determination of total polysaccharide content and analysis of monosaccharide components in the caulis polygoni multiflori mixture |
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| Abstract:Objective To establish a method for analyzing total polysaccharide content and its monosaccharide composition in the caulis polygoni multiflori mixture.Methods The polysaccharides of the caulis polygoni multiflori mixture were extracted by water-extraction and alcohol-precipitation. After the treatment with phenol-sulfuric acid, the content of total polysaccharides in the preparation was determined by ultraviolet spectrophotometry. In addition, after the polysaccharide was hydrolyzed into monosaccharides wtih trifluoroacetic acid, the hyrolysate was derivatized with PMP, and then the PMP derivates of monosaccharides were analyzed by HPLC method. Yilite krosmasil C18(4.6 mm×250 mm, 5 μm) was used at 30 ℃. Acetonitrile-0.1% NaH2PO4 (pH=6.8) (16:84) was the moblie phase with a flow rate of 1.0 ml/min. The detecting wavelength was at 250 nm. The injection volume was 20 μl.Results concentration of D-anhydrous glucose in the range of 21 ~ 105 μg/ml had a good linear relationship with the absorbance. The linear regression equation was A= 0.007x+0.0105, r=0.9982. The average recovery rate was (100.45±1.57)% (n=6). The average contents of total polysaccharides in four batches of samples were 14.24, 21.09, 17.85 and 18.17 mg/ml. The polysaccharide of the caulis polygoni multiflori mixture mainly consisted of D-mannose, D-glucosamine D-hydrochloride, D-Galacturonic acid, D-glucose, galactose, L-arabinose. The monosaccharides peak area ratios were about 9.10:0.26:1.00:3.02:4.14:2.12.Conclusion The method is accurate and reliable, and can be used for the determination of total content of polysaccharides and the analysis of monosaccharide composition in the preparation. |
| keywords:caulis polygoni multiflori mixture total polysaccharides ultraviolet spectrophotometry monosaccharide HPLC |
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