Page 31 - 《中国药房》2020年22期

何首乌九蒸九晒炮制工艺的优化研究 Δ

蒲俊安 ，张思敏 ，刘梦娇 ，肖望重 ，杨 磊 （1.湖南中医药大学第一附属医院药学教研室，长沙 410007；
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2.湖南中医药大学第一附属医院制剂中心，长沙 410007；3.湖南中医药大学第一附属医院全国名老中医药专
家张志国传承工作室，长沙 410007）
中图分类号 R283.3 文献标志码 A 文章编号 1001-0408（2020）22-2713-07
DOI 10.6039/j.issn.1001-0408.2020.22.05

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0.27～2.7 µg
（r＝0.997 1）、0.063～0.63 µg（r＝0.999 9）、0.038～0.38 µg（r＝0.990 9），总多糖检测质量浓度的线性范围为 2.07～12.42 µg/mL
（r＝0.999 6）；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4.5 h、烘制时间9 h、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。
关键词 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

Study on Optimization of the Nine-time Repeat Steaming and Sun-drying Process Processing Technology of
Polygonum multiflorum
PU Jun’an ，ZHANG Simin ，LIU Mengjiao ，XIAO Wangzhong ，YANG Lei （1. Pharmacy Teaching and
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Research Section，the First Affiliated Hospital of Hunan University of TCM，Changsha 410007，China；
2. Preparation Cener，the First Affiliated Hospital of Hunan University of TCM，Changsha 410007，China；
3. Zhang Zhiguo Heritage Studio of the Old Chinese Medicine Experts，the First Affiliated Hospital of Hunan
University of TCM，Changsha 410007，China）
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.
KEYWORDS Polygonum multiflorum； Nine-time repeat
Δ 基金项目：国家自然科学基金资助项目（No.81804075）；湖南省
steaming and sun-drying process；Central composite design-
自然科学基金资助项目（No.2017JJ3247） response surface methodology； HPLC； UV spectrometry；
＊硕士研究生。研究方向：中药炮制学。电话：0731-85600467。
Processing technology； Content determination； Technology
E-mail：741225040@qq.com
# 通信作者：副主任药师，副教授，硕士生导师，博士。研究方向： optimization
中药炮制学。电话：0731-85600467。E-mail：yanglei30@sohu.com

中国药房 2020年第31卷第22期 China Pharmacy 2020 Vol. 31 No. 22 ·2713 ·