不同月份杜仲叶中绿原酸含量分析及提取工艺研究
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摘要
以汉中地区杜仲叶为原料,对杜仲叶中绿原酸的累积规律及提取工艺进行了研究,以期为工业化生产提供理论依据,研究结果如下:
(1)采用高效液相色谱法对不同月份杜仲叶中绿原酸的含量进行了测定,结果表明在杜仲叶的生长周期中绿原酸的累积呈规律性变化,6月份绿原酸含量最高(2.22%),之后呈下降趋势,9月下降比较明显(1.138%),12月含量最低(0.826%)。
(2)不同保存方式对杜仲叶中绿原酸含量的影响较大。杜仲叶阴干,经室温保存一年后,绿原酸含量降低66.25%~50.08%。但新鲜杜仲叶经烘干低温冷藏5个月后,绿原酸含量基本没有变化。
(3)分别以水、乙醇为溶剂,在单因素实验的基础上,对绿原酸提取工艺条件进行正交实验;并采用中心组合设计,利用响应面分析法优化了杜仲叶中绿原酸水提工艺。水提正交实验最佳提取工艺条件为:料液比1:12,提取温度70℃,pH5,提取次数3次,每次1h,提取率为80.4%;醇提正交实验最佳提取工艺为:60%乙醇,料液比1:12,提取温度60℃,提取3次,每次1h,提取率为94.3%;响应面分析法优化水提工艺的最佳条件为:料液比1:16、提取温度65℃、提取次数2次、提取时间20min,提取率为92.46%。通过三种提取工艺的比较,结合经济成本综合考虑,得出最佳提取工艺为响应面分析法确定的水提工艺。
In order to provide a theoretical basis for industrial production.of chlorgenic acid, leaves of Eucommia ulmoides Olive.from Hanzhong Area were chosen as raw materials, which were used to study the accumulation rules and extraction methods of chlorgenic acid. The results were briefed as follows:
(1) The content of chlorgenic acid from Eucommia ulmoides Olive leaves in different months was assayed by high performance liquid chromatography. The result showed that the chlorgenic acid presented regular changes during the growth cycle of Eucommia ulmoides Olive leaves. The content of chlorgenic acid was highest in June(2.22%), then decreased gradually(1.138%), and then sharply decreased in September, (0.826%) reached minimum in December.
(2) Different storage methods play an important role in the contene of chlorgenic acid from Eucommia ulmoides Olive leaves. After the Eucommla ulmoides Olive leaves were dried in a shady place and kept in room temerature for a year, the content of chlorgenic acid was decreased by 66.25%~50.08%. However, The dried Eucommla ulmoides Olive leaves was kept under refrigeration condition for 5 months and the content of chlorgenic acid was substantially unchanged.
(3) The orthogonal test was performed to detect the extractive technology of Chlorgenic Acid from eucommla ulmoides Olive leaves using water and alcohol as solvent on the basis of single factor test. Moreover, the extractive technology was optimized by central composite design and respone surface analysis. Optimized conditions of water extracting chlorogrnic acid were as follows. The leaves were extracted with water of pH 5 at a ration of 1:12, and taken three times at 70℃for 60 min. The extraction rate of chlorogrnic acid was 80.4%. Optimized orthogonal test conditions of ethanol process were as following. The leaves were extracted with 60% ethanol of pH 5.0 at a ration of 1:12, and taken three times at 60℃for 60 min. The extraction rate of chlorogrnic acid was 94.3%. Optimized respone surface analysis conditions of water extracting chlorogrnic acid were as follows. The leaves were extracted at ration of 1:16, and taken two times at 65℃for 20 min.The extraction rate of chlorogrnic acid was 92.46%. Camparing the three extraction process with each other, we considered that the the optimized extraction process of chlorgenic acid from Eucommla ulmoides Olive leaves was respone surface analysis.
(1)采用高效液相色谱法对不同月份杜仲叶中绿原酸的含量进行了测定,结果表明在杜仲叶的生长周期中绿原酸的累积呈规律性变化,6月份绿原酸含量最高(2.22%),之后呈下降趋势,9月下降比较明显(1.138%),12月含量最低(0.826%)。
(2)不同保存方式对杜仲叶中绿原酸含量的影响较大。杜仲叶阴干,经室温保存一年后,绿原酸含量降低66.25%~50.08%。但新鲜杜仲叶经烘干低温冷藏5个月后,绿原酸含量基本没有变化。
(3)分别以水、乙醇为溶剂,在单因素实验的基础上,对绿原酸提取工艺条件进行正交实验;并采用中心组合设计,利用响应面分析法优化了杜仲叶中绿原酸水提工艺。水提正交实验最佳提取工艺条件为:料液比1:12,提取温度70℃,pH5,提取次数3次,每次1h,提取率为80.4%;醇提正交实验最佳提取工艺为:60%乙醇,料液比1:12,提取温度60℃,提取3次,每次1h,提取率为94.3%;响应面分析法优化水提工艺的最佳条件为:料液比1:16、提取温度65℃、提取次数2次、提取时间20min,提取率为92.46%。通过三种提取工艺的比较,结合经济成本综合考虑,得出最佳提取工艺为响应面分析法确定的水提工艺。
In order to provide a theoretical basis for industrial production.of chlorgenic acid, leaves of Eucommia ulmoides Olive.from Hanzhong Area were chosen as raw materials, which were used to study the accumulation rules and extraction methods of chlorgenic acid. The results were briefed as follows:
(1) The content of chlorgenic acid from Eucommia ulmoides Olive leaves in different months was assayed by high performance liquid chromatography. The result showed that the chlorgenic acid presented regular changes during the growth cycle of Eucommia ulmoides Olive leaves. The content of chlorgenic acid was highest in June(2.22%), then decreased gradually(1.138%), and then sharply decreased in September, (0.826%) reached minimum in December.
(2) Different storage methods play an important role in the contene of chlorgenic acid from Eucommia ulmoides Olive leaves. After the Eucommla ulmoides Olive leaves were dried in a shady place and kept in room temerature for a year, the content of chlorgenic acid was decreased by 66.25%~50.08%. However, The dried Eucommla ulmoides Olive leaves was kept under refrigeration condition for 5 months and the content of chlorgenic acid was substantially unchanged.
(3) The orthogonal test was performed to detect the extractive technology of Chlorgenic Acid from eucommla ulmoides Olive leaves using water and alcohol as solvent on the basis of single factor test. Moreover, the extractive technology was optimized by central composite design and respone surface analysis. Optimized conditions of water extracting chlorogrnic acid were as follows. The leaves were extracted with water of pH 5 at a ration of 1:12, and taken three times at 70℃for 60 min. The extraction rate of chlorogrnic acid was 80.4%. Optimized orthogonal test conditions of ethanol process were as following. The leaves were extracted with 60% ethanol of pH 5.0 at a ration of 1:12, and taken three times at 60℃for 60 min. The extraction rate of chlorogrnic acid was 94.3%. Optimized respone surface analysis conditions of water extracting chlorogrnic acid were as follows. The leaves were extracted at ration of 1:16, and taken two times at 65℃for 20 min.The extraction rate of chlorogrnic acid was 92.46%. Camparing the three extraction process with each other, we considered that the the optimized extraction process of chlorgenic acid from Eucommla ulmoides Olive leaves was respone surface analysis.
引文
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