CN113713423A - 一种超临界萃取制备黑豆馏油的工艺和应用 - Google Patents
一种超临界萃取制备黑豆馏油的工艺和应用 Download PDFInfo
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Abstract
本发明提供了一种超临界萃取制备黑豆馏油的工艺，将黑豆干燥粉碎，进行超临界二氧化碳萃取，得到黑豆溜油；在本发明中，所述萃取的温度为60℃，萃取的时间为4h，萃取的压力为45MPa，在此萃取条件下，萃取率达到15.3％，黑豆溜油的颜色为黄绿色，无明显臭味，且将油脂、酮类化合物、酰胺类、杂环类化合物等均萃取出来。通过与Ve的抗氧化性比较本方法制备得到的黑豆馏油具有较强的清除羟自由基和DPPH能力，萃取出来的成分具有较好的消炎、杀菌功效；再结合油脂的保护、润滑作用，能够很好的用于皮肤类药物成分添加。
Description
技术领域
本发明属于黑豆馏油的萃取工艺，尤其涉及一种超临界萃取制备黑豆馏油的工艺和应用。
背景技术
黑豆馏油为豆科植物黑大豆的种子，经干馏而得的黑色粘稠液体，具有消炎、收敛、止痒、使角质再生的功能，对于各类皮肤病有显著疗效。
由于传统的干馏法，制备温度高，导致其产品浓黑焦臭、清洗困难、气味浓重，限制了其功效成分的开发利用。
发明内容
有鉴于此，本发明的目的在于提供一种超临界萃取制备黑豆馏油的工艺和应用，该工艺萃取率高。
本发明提供了一种超临界萃取制备黑豆馏油的工艺，包括以下步骤：
将黑豆干燥粉碎，进行超临界二氧化碳萃取，得到黑豆溜油；
所述萃取的温度为55～65℃，萃取的时间为3.5～4.5h，萃取的压力为40～50MPa。
CO2流体超临界萃取是一种将超临界流体作为萃取剂，把一种成分从混合物中分离出来的技术。由于全过程不用有机溶剂，因此萃取物绝无残留溶媒，同时也防止了提取过程对人体的毒害和对环境的污染。CO2价格便宜，纯度高，容易取得，且在生产过程中循环使用，从而降低成本。
在本发明中，所述萃取的温度为60℃，萃取的时间为4h，萃取的压力为45MPa。
在本发明中，所述黑豆溜油中包括(E)-2-庚烯醛、2-氨基-N-(1H-四唑-5-基)苯甲酰胺、苯乙酮、丙二醇、3-羟基-3-苯基丁烷-2-酮、苯甲酸甲酯、壬醛、2-壬烯醛、煤焦油脑、7-己基二十烷-、(E)-2-癸烯醛、2,4-癸二烯醛、(E,E)-2,4-癸二烯醛、十四碳烷、邻苯二甲酸二甲酯、1,2-苯二甲酸二甲酯、1,2-苯二甲酸、十六烷酸、二十烷酸、8,11-十八烯酸、9-十八烯酸、硬脂酸甲酯、9,12-十八二烯酸、6-十八烯酸、十六酰胺、9-十八碳烯酰胺、硬脂酸酰胺、孕甾二醇和邻苯二甲酸二辛酯。
在本发明中，所述黑豆溜油的颜色为黄绿色。
本发明提供了一种由上述技术方案所述工艺制备的黑豆馏油在制备消炎药物、杀菌药物或皮肤类药物中的应用。
本发明提供了一种超临界萃取制备黑豆馏油的工艺，包括以下步骤：将黑豆干燥粉碎，进行超临界二氧化碳萃取，得到黑豆溜油；所述萃取的温度为55～65℃，萃取的时间为3.5～4.5h，萃取的压力为40～50MPa。本发明采用超临界流体萃取技术制备黑豆馏油，在上述萃取条件下，萃取率较高，且将油脂、酮类化合物、酰胺类、杂环类化合物等均萃取出来。萃取出来的成分具有较好的消炎、杀菌功效；再结合油脂的保护、润滑作用，能够很好的用于皮肤类药物成分添加。
附图说明
图1为超临界萃取装置示意图；
图2为为温度为萃取率的影响；
图3为萃取时间对萃取率的影响；
图4为萃取压力对萃取率的影响；
图5为实施例1的总离子流图；
图6为Ve与黑豆馏油DPPH清除率对比图；
图7为Ve和黑豆馏油羟自由基清除率对比图；
图8为Ve与黑豆馏油超氧阴离子清除率对比例图。
具体实施方式
为了进一步说明本发明，下面结合实施例对本发明提供的一种超临界萃取制备黑豆馏油的工艺和应用进行详细地描述，但不能将它们理解为对本发明保护范围的限定。
以下实施例和对比例均采用图1所示的超临界萃取装置示意图；其中，A代表CO2贮罐，B为净化器，C为冷循环装置，D为高压泵，E为萃取缸，F为分离器Ⅰ，G为分离器Ⅱ；1，2，3，4，5和6均代表阀门；
实施例1
本发明采用响应面试验设计对CO2流体超临界萃取黑豆馏油工艺进行优化，制备的黑豆馏油通过气质联用进行成分分析：
1)单因素试验设计
采用单因素试验对影响黑豆馏油萃取率的超临界萃取工艺条件进行筛选和分析，根据参考资料，对黑豆的萃取压力、萃取温度、萃取时间进行实验设计：
萃取温度对黑豆馏油的萃取率影响，见图2，图2为温度为萃取率的影响；由图1可知，温度从50℃升高到65℃时，黑豆馏油的萃取率随温度的上升呈明显上升趋势；因此响应面实验的萃取温度水平范围为55、60、65℃。
图3为萃取时间对萃取率的影响；由图3可知，随着萃取时间延长，黑豆馏油萃取率增加明显，但延长至4h后，增加波动幅度不大。考虑到随时间延长，机器及各方面消耗越大，因此确定响应面实验的萃取时间水平为2、3、4h
图4为萃取压力对萃取率的影响。由图4可知，压力从30MPa上升至35MPa时，黑豆馏油萃取率大幅度增加随之增加到40MPa时，萃取率明显减少；当压力上升至45MPa，黑豆馏油萃取率的波动极小，所以从经济和安全方面综合考虑，响应面实验的萃取压力水平选择35MPa、40MPa、45MPa。
2)响应面试验设计
根据单因素试验，选定A(萃取压力)、B(萃取温度)、C(萃取时间)3个考察因素及其变化水平，设计3因素3水平共17个试验点的响应面试验设计方案,建立数学回归模型，反映不同因素之间的交互影响，以松针挥发油提取率为评价的指标，响应面试验结果及方差分析。响应面实验设计如下表1所示：
表1超临界流体萃取黑豆馏油工艺响应面试验因素水平表
3)气质联用分析黑豆馏油成分
气相色谱条件:
HP-5(聚二甲基硅氧烷)石英毛细管柱(30m×0.20mm×0.33μm)程序升温:炉温40℃保持6min，8℃/min升至260℃。进样口温度250℃，载气为氮气，进样量1μL。质谱条件:电子轰击(EI)，电子能量70eV，传输线温度250℃，离子源温度260℃，电子倍增器电压240V，扫描范围20～500amu。
4)超临界萃取制备黑豆馏油的工艺优化：
以黑豆馏油提取率为评价的指标，响应面试验结果及方差分析见表2和表3。
表2响应面试验结果
表3方差分析
采用响应面试验设计建立模型优化超临界萃取黑豆馏油工艺。通过自变量和因变量得到一个在给定范围内预测响应值的回归方程：
萃取率＝+13.52+1.65*A+0.78*B+1.40*C+0.000*A*B-0.80*A*C-0.60*B*C-1.04*A2-1.24*B2+0.22*C2
得到模型的决定系数为0.9664。从表3中可以看出，就所得回归方程模型(p＜0.001)，可充分表明3个因素之间关系。在给定水平范围内，萃取温度、萃取时间和萃取压力均为影响黑豆馏油萃取率明显的要素，其中萃取压力对黑豆馏油萃取率的影响最大，萃取时间次之，萃取温度最小。根据建立的数学模型进行参数最优化分析，超临界萃取黑豆馏油最佳参数条件为：萃取温度60℃、萃取时间4h、萃取压力45MPa，在此条件下萃取率模型的预测值为13.52％，实际得到的萃取率为15.3％。
5)本发明萃取得到的黑豆馏油成分分析：
通过气质联用对最佳条件得到的黑豆馏油成分进行了分析，总离子流图(见图5)及表4可以看出采用气质联用分析黑豆馏油，得到了29种成分，根据图库及文献查阅主要为脂肪酸、酮、醛、酯及酰胺类成分，与干馏法制备的黑豆馏油成分相似。通过超临界萃取的黑豆馏油颜色呈现黄绿色，焦臭味道明显降低，大大改善了干馏法制备黑豆馏油的品质。
表4实施例1制备的黑豆馏油成分分析结果
对比例1
与实施例1不同的是，萃取温度为30℃，时间为2h，萃取压力为25MPa。在此条件下实际得到的萃取率为9.1％。
通过气质联用对得到的黑豆馏油成分进行了分析，见表5：
表5对比例1制备的黑豆馏油的成分分析结果
由表5可以看出：黑豆馏油主要是黄色组分，为油脂部分，相比本发明，没有酮类、烷烃类等组分。
对比例2
采用传统干馏法(温度200℃以上)制备黑豆馏油。萃取率为29.6％。
通过气质联用对得到的黑豆馏油成分进行了分析，见表6：
表6对比例2制备的黑豆馏油的成分分析结果
由表6可知，干馏法制得的黑豆馏油，得到了18种组分，根据图库及文献查阅主要为烷烃、醛及酮类成分，相比本发明，缺少了油脂及脂肪酸类成分。
本发明对实施例1和对比例1及对比例2制得的黑豆馏油进行抗氧化性能测试：
抗氧化测试方法：将三种方法制备的黑豆馏油浓度调整到1.0mg/mL，然后分别稀释5倍、10倍、50倍、100倍、500倍，与Ve进行抗氧化性比较。
1.DPPH自由基清除试验
采用Ve为对照组。
2.清除·OH自由基的作用
采用Fenton试剂法检测样品对羟自由基的清除作用，同时采用Ve为对照组。
3.清除超氧阴离子的作用
采用邻苯三酚自氧化法测定样品对超氧阴离子的清除作用，同时采用Ve、为对照组。
抗氧化测试结果分别见图6、图7和图8：其中，图6为Ve与黑豆馏油DPPH清除率对比图；图7为Ve和黑豆馏油羟自由基清除率对比图；图8为Ve与黑豆馏油超氧阴离子清除率对比例图。由图6～图8可知，通过本方法制备的黑豆馏油对DPPH和羟自由基具有显著的清除效果，本实施例与对比例1和对比例2相比较，原浓度对DPPH清除率高达79.8％，高于对比例1的63.5％和对比例2的48.7％；原浓度对羟自由基的清除率高达95.3％，高于对比例1的91.5％和对比例2的83.2％；三种方法制备的黑豆馏油对超氧阴离子的清除效果与Ve相比不显著。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种超临界萃取制备黑豆馏油的工艺，包括以下步骤：
将黑豆干燥粉碎，进行超临界二氧化碳萃取，得到黑豆溜油；
所述萃取的温度为55～65℃，萃取的时间为3.5～4.5h，萃取的压力为40～50MPa。
2.根据权利要求1所述的工艺，其特征在于，所述萃取的温度为60℃，萃取的时间为4h，萃取的压力为45MPa。
3.根据权利要求1所述的工艺，其特征在于，所述黑豆溜油中包括(E)-2-庚烯醛、2-氨基-N-(1H-四唑-5-基)苯甲酰胺、苯乙酮、丙二醇、3-羟基-3-苯基丁烷-2-酮、苯甲酸甲酯、壬醛、2-壬烯醛、煤焦油脑、7-己基二十烷-、(E)-2-癸烯醛、2,4-癸二烯醛、(E,E)-2,4-癸二烯醛、十四碳烷、邻苯二甲酸二甲酯、1,2-苯二甲酸二甲酯、1,2-苯二甲酸、十六烷酸、二十烷酸、8,11-十八烯酸、9-十八烯酸、硬脂酸甲酯、9,12-十八二烯酸、6-十八烯酸、十六酰胺、9-十八碳烯酰胺、硬脂酸酰胺、孕甾二醇和邻苯二甲酸二辛酯。
4.根据权利要求1所述的工艺，其特征在于，所述黑豆溜油的颜色为黄绿色。
5.一种由权利要求1～4任一项所述工艺制备的黑豆馏油在制备消炎药物、杀菌药物或皮肤类药物中的应用。
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