止得咳颗粒提取工艺的优化
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篇名: 止得咳颗粒提取工艺的优化
TITLE: Optimization of the Extraction Technology of Zhideke Granules
摘要: 目的:优化止得咳颗粒的提取工艺。方法:采用小鼠氨水引咳实验和二甲苯致耳肿胀实验初步筛选止得咳颗粒的提取方法(水提、醇提、水提醇沉法)。基于该方的制备路线,首先以吸水量为指标,考察含挥发油药材的浸泡时间;再并以挥发油得率为指标,采用单因素试验考察加水量和提取时间,筛选含挥发油药材的最优提取工艺。以次野鸢尾黄素和总黄酮含量为指标,在单因素考察的基础上,采取正交试验考察加水量、提取时间、提取次数等3个因素的影响,优化止得咳颗粒的水提工艺并验证。结果:药效学实验结果显示,水提物低、高剂量组(6.34、12.68g/kg,以生药量计)和水提醇沉提取物高剂量组(12.68g/kg,以生药量计)小鼠的咳嗽潜伏期均较模型组显著延长,2min内咳嗽次数显著减少(P<0.05或P<0.01);水提物低、高剂量组(6.34、12.68g/kg,以生药量计),醇提物高剂量组(12.68g生药/kg,以生药量计)和水提醇沉提取物高剂量组(12.68g/kg,以生药量计)小鼠的耳肿胀度均较模型组显著降低(P<0.05或P<0.01),水提物、醇提物和水提醇沉提取物低、高剂量组的肿胀抑制率分别为42.26%、55.08%、33.49%、51.56%、39.57%、44.36%,表明以水提法所得提取物的止咳、抗炎效果更优。含挥发油药材的最优提取工艺为加入5倍量水,浸泡30min,提取3h。最佳水提工艺为加入12倍量水,浸泡50min后提取3次,每次1.0h;3次验证试验结果显示,最优工艺所得提取物中次野鸢尾黄素的平均含量为76.47μg/g(RSD=2.15%,n=3),总黄酮的平均含量为92.45mg/g(RSD=0.48%,n=3)。结论:优化的止得咳颗粒提取工艺稳定、可行。
ABSTRACT: OBJECTIVE:To optimize the extraction technology of Zhideke granules. ME THODS:The extraction technology (water extraction ,alcohol extraction ,water extraction and ethanol precipitation )of Zhideke granules was initially screened by ammonia-induced cough experiment and xylene-induced ear swelling experiment in mice. Based on its preparation route ,the immersion time of medicinal materials containing volatile oil was investigated with water absorption as index firstly. The single factor test was adopted to investigate the amount of water added and the extraction time taking the volatile oil yield as index to optimize the extraction technology of medicinal materials containing volatile oil. Taking the contents of irisflorentin and total flavonoids as indicators ,on the basis of single factor investigation ,orthogonal test was adopted to examine the influence of three factors including the amount of water added ,extraction time and extraction frequency ,so as to optimize the water extraction technology of Zhideke granules and the validation tests were conducted. RESULTS :The results of pharmacodynamics experiment showed that the cough latency of mice in water extract low-dose and high-dose groups (6.34,12.68 g/kg,by crude drug )and water-extraction alcohol-precipitation extract high-dose group (12.68 g/kg,by crude drug )were significantly longer than those inmodel group ,and the number of cough within 2 minutes was significantly reduced (P<0.05 or P<0.01). Compared with model group , the ear swelling of mice in water extract low-dose and high-dose groups (6.34,12.68 g/kg,by crude drug),ethanol extract high-dose group (12.68 g/kg,by crude drug) and water-extraction alcohol-precipitation extract hig dose group (12.68 g/kg,by crude drug ) were decreased significantly (P<0.05 or P<0.01). The swelling inhibition rates were 42.26%,55.08%,33.49%,51.56%,39.57% and 44.36% in low-dose and high-dose groups of water extract ,alcohol extract , water-extraction and alcohol-precipitation extract respectively ,indicating that the water extract had better antitussive and anti-inflammatory effects. The optimal extraction technology of volatile oil was adding 5-fold water ,soaking for 30 minutes,and extracting for 3 hours. The optimal water extraction technology was adding 12-fold water ,extracting for 3 times after soaked for 50 min,lasting for 1 h each time. Results of 3 times of validation tests showed that average content of irisflorentin in the extract obtained by optimal technology was 76.47 μg/g(RSD= 2.15%,n=3)and the average content of total flavonoids was 92.45 mg/g(RSD=0.48%,n=3). CONCLUSIONS :The optimal extraction technology of Zhideke granules is stable and feasible.
期刊: 2021年第32卷第07期
作者: 梁洁,陈辉华,徐晖,谢谭芳,祁静,信晨曦,陈日兰,赵立春
AUTHORS: LIANG Jie,CHEN Huihua ,XU Hui,XIE Tanfang ,QI Jing,XIN Chenxi ,CHEN Rilan,ZHAO Lichun
关键字: 止得咳颗粒;药效学;正交试验;提取工艺
KEYWORDS: Zhideke granules ;Pharmacodynamics;Orthogonal test ;Extraction technology
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