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Box-Behnken响应面法优化炒赤芍炮制工艺 Δ
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许天阳 ,董坤园 ,宋凤媛 ,钱 圳 ,熊金璐 ,于 澎 (1.长春中医药大学创新实践中心,长春 130117;2.长
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春中医药大学药学院,长春 130117)
中图分类号 R283.3 文献标志码 A 文章编号 1001-0408(2019)20-2845-06
DOI 10.6039/j.issn.1001-0408.2019.20.21
摘 要 目的:优化炒赤芍的炮制工艺,为该炮制品的质量控制提供参考。方法:采用高效液相色谱法对炒赤芍中的芍药苷进行
含量测定。色谱柱为 Agilent ZORBAX SB-C18,流动相为乙腈-0.05 mol/L 磷酸二氢钾溶液(15 ∶ 85,V/V),流速为 1.0 mL/min,柱
温为30 ℃,检测波长为230 nm,进样量为10 μL。以表面颜色、断面颜色、硬度、气味考察炒赤芍的外观性状;以外观性状评分和芍
药苷含量评分的综合评分为考察指标,分别对投药量、炒制温度、炒制时间进行单因素考察,并根据单因素试验结果对上述3个因
素进行Box-Behnken响应面法优化,并对优化后的炮制工艺进行验证。结果:芍药苷检测质量浓度的线性范围为0.02~4.15 mg/mL
(r=0.999 9);精密度、稳定性、重复性、加样回收率均符合要求。炒赤芍的最优工艺为投药量374.60 g、炒制温度101.61 ℃、炒制
时间 20 min。在最优工艺条件下,6 次平行验证试验所得炒赤芍的综合评分为 97.39~98.82 分,RSD 为 0.54%,与预测值(98.18
分)相接近;炒赤芍颜色较赤芍生品略有加深,质脆,有香味。结论:优化所得炒赤芍的炮制工艺稳定、可行,适用于该炮制品的
制备。
关键词 炒赤芍;芍药苷;外观性状;响应面法;Box-Behnken设计
Optimization of Processing Technology of Fried Radix Paeoniae by Box-Behnken Response Surface Method
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XU Tianyang ,DONG Kunyuan ,SONG Fengyuan ,QIAN Zhen ,XIONG Jinlu ,YU Peng (1. Innovation
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Practice Center, Changchun University of TCM, Changchun 130117, China; 2. College of Pharmacy,
Changchun University of TCM,Changchun 130117,China)
ABSTRACT OBJECTIVE:To optimize the processing technology of fried Radix Paeoniae,and to provide reference for quality
control of the processed products. METHODS:The content of paeoniflorin in fried Radix Paeoniae was determined by HPLC. The
determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of acetonitrile-0.05 mol/L potassium
dihydrogen phosphate solution(15 ∶ 85,V/V)at the flow rate of 1.0 mL/min. The column temperature was 30 ℃,and detection
wavelength was set at 230 nm. The sample size was 10 μL. The appearance character of fried Radix Peaoniae were investigated by
appearance color,crosssection color,hardness and smell. Taking the comprehensive score of appearance character and paeoniflorin
content as evaluation index,the dosage,stir-frying temperature and stir-frying time were investigated. According to the results of
single factor test,Box-Behnken response surface methodology was used to optimize above 3 factors. The optimized processing
technology was validated. RESULTS:The linear range of paeoniflorin were 0.02-4.15 mg/mL(r=0.999 9);precision,stablity,
repeatability and sample recovery rate meet the requirements. The optimal technology of fried Radix Paeoniae included the dosage
of 374.60 g,frying temperature of 101.61 ℃,frying time of 20 min. Under optimal technology,comprehensive score of fried
Radix Paeoniae ranged 97.39-98.82 in 6 times of parallel verification tests(RSD=0.54%),which was close to predicted value
98.18. The color of fried Radix Paeoniae was slightly deeper than Radix Paeoniae,which was crisp and fragrant. CONCLUSIONS:
The optimized processing technology of fried Radix Paeoniae is stable and feasible,and is suitable for the preparation of the
processed products.
KEYWORDS Fried Radix Paeoniae;Paeoniflorin;Appearance character;Response surface method;Box-Behnken design
赤芍为毛茛科植物芍药(Paeonia lactiflora Pall.)或 有34家药品生产企业生产参桂再造丸,其中吉林省有9
[1]
川赤芍(P. veitchii Lynch)的干燥根 。赤芍饮片炮制方 家 。但2015年版《中国药典》(一部)以及《吉林省中药
[2]
法包括炒赤芍、酒赤芍等,其中炒赤芍是舒经活络、祛风 炮制标准》(1986年版)中并未收载炒赤芍的炮制规范及
行血的常用药参桂再造丸的重要药味之一。目前,全国 质量标准,因此对于吉林省中药生产企业而言,炒赤芍
Δ 基金项目:吉林省中医药管理局中药特色技术传承人材培训项 尚无明确标准可依。《全国中药炮制规范》(1988年版)虽
目(No.吉中医药发〔2018〕159号);吉林省中医药管理局特色药材炮制 然规定炒赤芍为“取赤芍片置锅内,用文火加热,炒至颜
规范项目(No.PZ-2017-07) 色加深,偶有焦斑,取出放凉”,但具体工艺参数并不明
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*讲师,硕士。研究方向:中药分析、中药质量标准。电话:
确,仅以炮制品表面颜色判断炮制终点,无法有效控制
0431-86763972。E-mail:7809087@qq.com
# 通信作者:副教授,硕士。研究方向:中药炮制。电话:0431- 炒赤芍质量。本课题组在参与《吉林省中药饮片炮制规
86172207。E-mail:342905933@qq.com 范》编制项目过程中,尝试建立了炒赤芍的炮制规范与
中国药房 2019年第30卷第20期 China Pharmacy 2019 Vol. 30 No. 20 ·2845 ·