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何首乌九蒸九晒炮制工艺的优化研究
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| 篇名： | 何首乌九蒸九晒炮制工艺的优化研究 |
| TITLE： | Study on Optimization of the Nine-time Repeat Steaming and Sun-drying Process Processing Technology of Polygonum multiflorum |
| 摘要： | 目的：建立测定何首乌中二苯乙烯苷、大黄素、大黄素甲醚和总多糖含量的方法，并优化何首乌传统九蒸九晒的炮制工艺。方法：采用高效液相色谱法检测二苯乙烯苷、大黄素、大黄素甲醚的含量；采用紫外分光光度法检测总多糖的含量。以蒸制时间、烘制时间、烘制温度为自变量，二苯乙烯苷、大黄素、大黄素甲醚和总多糖含量为指标，结合加权综合评分法和星点设计-效应面法优化何首乌九蒸九晒的炮制工艺并验证。结果：二苯乙烯苷、大黄素、大黄素甲醚检测进样量的线性范围分别为0.27～2.7µg（r＝0.9971）、0.063～0.63µg（r＝0.9999）、0.038～0.38µg（r＝0.9909），总多糖检测质量浓度的线性范围为2.07～12.42µg/mL（r＝0.9996）；精密度、稳定性、重复性试验的RSD均小于2％；加样回收率分别为99.43％～101.06％（RSD＝0.63％，n＝6）、98.74％～120.33％（RSD＝1.34％，n＝6）、98.39％～102.44％（RSD＝1.49％，n＝6）、99.51％～101.98％（RSD＝0.87％，n＝6）。最优炮制工艺为蒸制时间4.5h、烘制时间9h、烘制温度66℃，反复炮制9次。3次验证试验结果显示，最优炮制工艺的平均综合评分为35.69分，与预测值（36.90分）的相对误差为3.30％。结论：所建含量测定方法操作简便、重复性好；优化所得炮制工艺预测性良好且稳定、可行。 |
| ABSTRACT： | OBJECTIVE：To establish methods for the content determination of stilbene glycoside ，emodin，emodin methyl ether and total polysaccharide in P. multiflorum ，and to optimize the processing technology of traditional nine-time repeat steaming and sun-drying process of P. multiflorum . METHODS ：HPLC method was adopted to determine the contents of stilbene glycoside ， emodin，and emodin methyl ether. The content of total polysaccharide was determined by UV spectrometry. With steaming time ， drying time and drying temperature as independent variables ，the contents of stilbene glycoside ，emodin，emodin methyl ether and total polysaccharide as indexes ，the processing technology of nine-time repeat steaming and sun-drying process of P. multiflorum was optimized by weighted comprehensive score method and central composite design-response surface method ，and the validation tests were conducted. RESULTS ：The linear range of sample size of stilbene glycoside ，emodin and emodin methyl ether were 0.27-2.7 µg（r＝0.997 1），0.063-0.63 µg（r＝0.999 9），0.038-0.38 µg（r＝0.990 9），respectively. The linear range of mass concentration of total polysaccharide was 2.07-12.42 µg/mL（r＝0.999 6），respectively. RSDs of precision ，stability and reproducibility tests were all lower than 2％. The recoveries were 99.43％-101.06％（RSD＝0.63％，n＝6），98.74％-120.33％ （RSD＝1.34％，n＝6），98.39％-102.44％（RSD＝1.49％，n＝6），99.51％-101.98％（RSD＝0.87％，n＝6），respectively. The optimal processing technology was steaming time for 4.5 h，drying time for 9 h，drying temperatrue for 66 ℃ and repeat processing for 9 times. Results of 3 times of validation tests showed that the comprehensive score of optimal technology was 35.69， relative error of which to predicted value （36.90）was 3.30％. CONCLUSIONS ：Established method is simple and reproducible ， and the optimal processing technology is predicive ，stable feasible. |
| 期刊： | 2020年第31卷第22期 |
| 作者： | 蒲俊安，张思敏，刘梦娇，肖望重，杨磊 |
| AUTHORS： | PU Jun ’an，ZHANG Simin，LIU Mengjiao，XIAO Wangzhong，YANG Lei |
| 关键字： | 何首乌；九蒸九晒；星点设计-效应面法；高效液相色谱法；紫外分光光度法；炮制工艺；含量测定；工艺优化 |
| KEYWORDS： | Polygonum multiflorum； Nine-time repeat |
| 阅读数： | 545 次 |
| 本月下载数： | 3 次 |
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