博落回和鬼针草有效成分的提取工艺研究
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摘要
中药有着悠久的历史,由于其组成成分较复杂,需要用合适的提取方法将原料中的有效成分提取出来。因此提取是中药制药的关键环节,影响着最终药物制剂的质量和成本,以及重要制药业的现代化水平。本文介绍了传统提取法,包括：煎煮法、浸渍法、渗漉法、回流提取法、水蒸气蒸馏法；和现代提取方法,包括：超临界流体萃取、微波萃取、超声波提取、酶法提取、半仿生提取等技术的原理和特点,以及这些传统法和现代提取法在中药研究中的应用。重点介绍了新型的内部沸腾法,考察了操作压力、提取温度及提取时间对其的影响；该法与传统法和现代提取法相比具有提取时间短,提取温度低,得率高等优点。本文以博落回和鬼针草植物为原料,分别用传统法和内部沸腾法提取两者中的植物有效成分,并将两种方法的提取结果加以比较。
首先,本文建立了高效液相色谱法分析博落回总碱中血根碱的分析方法,采用最适合本体系的高效液相色谱条件：C18柱,流动相为乙腈/0.2%磷酸水溶液=25/75(V/V),柱温为25℃,流速为1.0mL/min,检测波长为282nm。由于博落回总生物碱的成分较复杂,主要考察博落回血根碱的含量,绘制了血根碱的含量标准曲线：Y=8.2903+875.55X,线性良好(R2=0.99503)。
其次,用乙醇作为提取溶剂研究了博落回和鬼针草有效成分的提取工艺,通过实验考察得到的较优提取工艺为：乙醇浓度70%(V/V),提取温度60℃,液固比10:1,提取时间3h,在此提取工艺条件下,血根碱提取得率为20.89mg/g。比较了不同部位的原料(叶部、茎部、根部)的提取,实验结果表明：叶部的提取得率最大,依次是茎部和根部。
最后,用内部沸腾法研究了博落回和鬼针草有效成分的提取,考察了内部沸腾法的主要两步：解吸过程与减压过程。确定了本实验的较优提取工艺条件：解吸剂浓度为90%乙醇溶液(V/V)、解吸时间为20min、解吸剂用量为50mL、提取温度为50℃、操作压力为-70kPa、提取时间为30min,在较优的提取工艺条件下,血根碱提取得率为26.95mg/g。取三种原料的不同部位(叶部、茎部、根部)在内部沸腾法较优的工艺条件下提取,结果表明：叶部的血根碱提取得率最大,依次是茎部和根部。与传统法相比,内部沸腾法在提取温度低10℃,提取时间少5倍的前提下,提取得率仍大于传统法；与现代提取法相比,内部沸腾法具有对设备要求低,能耗低的特点,因此内部沸腾法具有广泛的工业应用前景。
Traditional Chinese medicine has a long history in China. Because of complex composition, it requires appropriate extraction method to extract the active ingredients from raw material. The extraction is the key operation step in the production of Chinese material medical or the natural products. This article reviews several traditional extract methods such as impregnation, boiling method, percolation method, reflux extraction and distillation extraction and modern extract methods like supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), enzymatic extraction (ETE) and semi-bionic extraction (SBE). The principle, characteristics and the application of these technologies in traditional Chinese medicine research were introduced. As a new method, inner ebullition extraction was studied. The effects of pressure, temperature and extracting time on extraction of active ingredient were discussed. Compared with other extraction methods, inner ebullition extraction was found to be a faster and more effective method with lower extracting temperature, shorter extracting time and higher extraction yield. The article investigated the processes for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with traditional method and inner ebullition method.
Firstly, a HPLC method was established for the determination of sanguinarine in Macleaya cordata. HPLC analysis was carried out on C18 column and the acetonitrile-0.2% phosphoric acid solution(25:75) as the mobile phase, the column temperature at 25℃, the flow rate at 1.0 mL/min and the detection wavelength at 282nm. Because of complex composition, concentration of sanguinarine was determined to reflect total alkaloids in Macleaya cordata. Regression equation is Y=8.2903+875.55X, correlation coefficient R2=0.99503.
Secondly, the process for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with ethanol was studied. The extraction yield of sanguinarine was 20.89mg/g under the optimum condition when using the concentration of ethanol 70%(V/V), the extraction temperature at 60℃, the ratio of solvent to material at 10, the extraction time for 3h. Comparison of different parts of raw material, experimental showed that the extraction yield of sanguinarine decreased in the order of the leaves, the stems and the roots.
Finally, the process for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with inner ebullition method was studied. Inner ebullition method included saturating process and decompressing process. The optimum condition of ethanol extraction was that:the concentration of releasing solvent ethanol 90%(V/V), the saturating time for 20min, the volume of resolution of 50 mL, the extraction temperature at 50℃, the extraction pressure under-70kPa, the extraction time for 30min. Using this technology, the extraction yield of sanguinarine was 26.95mg/g. Comparison of different parts of raw material, experimental showed that the extraction yield of sanguinarine decreased in the order of the leaves, the stems and the roots. Compared with traditional method, this method has lower extracting temperature, shorter extracting time and higher extraction yield. Compared with modern extracting methods, this method doesn't need complex extracting devices and avoid high energy consumption.
首先,本文建立了高效液相色谱法分析博落回总碱中血根碱的分析方法,采用最适合本体系的高效液相色谱条件：C18柱,流动相为乙腈/0.2%磷酸水溶液=25/75(V/V),柱温为25℃,流速为1.0mL/min,检测波长为282nm。由于博落回总生物碱的成分较复杂,主要考察博落回血根碱的含量,绘制了血根碱的含量标准曲线：Y=8.2903+875.55X,线性良好(R2=0.99503)。
其次,用乙醇作为提取溶剂研究了博落回和鬼针草有效成分的提取工艺,通过实验考察得到的较优提取工艺为：乙醇浓度70%(V/V),提取温度60℃,液固比10:1,提取时间3h,在此提取工艺条件下,血根碱提取得率为20.89mg/g。比较了不同部位的原料(叶部、茎部、根部)的提取,实验结果表明：叶部的提取得率最大,依次是茎部和根部。
最后,用内部沸腾法研究了博落回和鬼针草有效成分的提取,考察了内部沸腾法的主要两步：解吸过程与减压过程。确定了本实验的较优提取工艺条件：解吸剂浓度为90%乙醇溶液(V/V)、解吸时间为20min、解吸剂用量为50mL、提取温度为50℃、操作压力为-70kPa、提取时间为30min,在较优的提取工艺条件下,血根碱提取得率为26.95mg/g。取三种原料的不同部位(叶部、茎部、根部)在内部沸腾法较优的工艺条件下提取,结果表明：叶部的血根碱提取得率最大,依次是茎部和根部。与传统法相比,内部沸腾法在提取温度低10℃,提取时间少5倍的前提下,提取得率仍大于传统法；与现代提取法相比,内部沸腾法具有对设备要求低,能耗低的特点,因此内部沸腾法具有广泛的工业应用前景。
Traditional Chinese medicine has a long history in China. Because of complex composition, it requires appropriate extraction method to extract the active ingredients from raw material. The extraction is the key operation step in the production of Chinese material medical or the natural products. This article reviews several traditional extract methods such as impregnation, boiling method, percolation method, reflux extraction and distillation extraction and modern extract methods like supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE), enzymatic extraction (ETE) and semi-bionic extraction (SBE). The principle, characteristics and the application of these technologies in traditional Chinese medicine research were introduced. As a new method, inner ebullition extraction was studied. The effects of pressure, temperature and extracting time on extraction of active ingredient were discussed. Compared with other extraction methods, inner ebullition extraction was found to be a faster and more effective method with lower extracting temperature, shorter extracting time and higher extraction yield. The article investigated the processes for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with traditional method and inner ebullition method.
Firstly, a HPLC method was established for the determination of sanguinarine in Macleaya cordata. HPLC analysis was carried out on C18 column and the acetonitrile-0.2% phosphoric acid solution(25:75) as the mobile phase, the column temperature at 25℃, the flow rate at 1.0 mL/min and the detection wavelength at 282nm. Because of complex composition, concentration of sanguinarine was determined to reflect total alkaloids in Macleaya cordata. Regression equation is Y=8.2903+875.55X, correlation coefficient R2=0.99503.
Secondly, the process for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with ethanol was studied. The extraction yield of sanguinarine was 20.89mg/g under the optimum condition when using the concentration of ethanol 70%(V/V), the extraction temperature at 60℃, the ratio of solvent to material at 10, the extraction time for 3h. Comparison of different parts of raw material, experimental showed that the extraction yield of sanguinarine decreased in the order of the leaves, the stems and the roots.
Finally, the process for extracting active ingredient from Macleaya cordata and Bidens bipinnata L with inner ebullition method was studied. Inner ebullition method included saturating process and decompressing process. The optimum condition of ethanol extraction was that:the concentration of releasing solvent ethanol 90%(V/V), the saturating time for 20min, the volume of resolution of 50 mL, the extraction temperature at 50℃, the extraction pressure under-70kPa, the extraction time for 30min. Using this technology, the extraction yield of sanguinarine was 26.95mg/g. Comparison of different parts of raw material, experimental showed that the extraction yield of sanguinarine decreased in the order of the leaves, the stems and the roots. Compared with traditional method, this method has lower extracting temperature, shorter extracting time and higher extraction yield. Compared with modern extracting methods, this method doesn't need complex extracting devices and avoid high energy consumption.
引文
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