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
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