CN108354146A - 一种生姜中活性物质的综合提取工艺 - Google Patents
一种生姜中活性物质的综合提取工艺 Download PDFInfo
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Abstract
本发明公开了一种生姜中活性物质的综合提取工艺。本发明工艺采用微波辅助提取工艺提取生姜精油，并对生姜精油提取后剩余物进一步提取活性物质，通过加热水提、醇沉等技术，进一步获得生姜不溶性膳食纤维粗提物、生姜抗氧化剂和生姜多糖。本发明工艺综合提取的四种活性物质得率理想，并且不含有毒有害溶剂，符合食品原料要求，可用于高附加值产品的开发生产，将生姜精油提取后的剩余物回收利用，不仅能增加生产企业的经济效益，还可减轻废弃物排放造成的环境污染，其市场前景广阔且具有重大的社会意义。
Description
技术领域
本发明属于生物活性物质提取领域，更具体的，涉及一种生姜中活性物质的综合提取工艺。
背景技术
姜为多年生草本植物，供食用的部分是肥大的根茎，可一种二收，早秋收嫩姜，深秋收老姜。姜是一种极为重要的调味品，还是一味重要的中药材，有生发作用，也是心血管系统的有益保健品。
中医认为，姜性温，味辣，具有发表散寒、温肺止咳、温胃止呕、解毒止泻、调味等功效。姜能增强血液循环，有刺激胃液分泌、兴奋肠管、促进消化、增进食欲的作用；有排汗、降温、提神的作用，可缓解疲劳、乏力、厌食、失眠、腹胀、腹痛等症状；可用于治疗风寒感冒、呕吐泄泻、痰饮喘咳等症；可用于鱼蟹、禽兽肉等食物中毒的解毒；还有助于预防晕船和晕车。
姜主要含有姜醇、姜油萜、姜烯、水芹烯、柠檬醛、芳香油等油性挥发物，还有姜辣素、维生素、姜油酚、树脂、淀粉、纤维及少量的矿物质，因此从生姜中提取活性物质，用于高附加值产品的开发生产，具有非常重要的意义。
发明内容
本发明的目的在于提供一种生姜中活性物质的综合提取工艺。
本发明所采取的技术方案是：
一种生姜中活性物质的综合提取工艺，包括如下制备步骤：
(1)将新鲜的生姜清洗干净，切块，搅成泥状；
(2)将步骤(1)获得的泥状生姜与水混合，用微波辅助提取，分离，获得生姜精油和剩余物；
(3)将剩余物加热水提，离心，获得水提液A和残渣，将残渣干燥，获得生姜不溶性膳食纤维粗提物；
(4)水提液A用乙醇醇沉，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
作为上述工艺的优选，步骤(1)中，切块后加入乙醇，乙醇的添加量为生姜重量的1～10％。
作为上述工艺的优选，步骤(2)中，泥状生姜与水按质量体积比为5g：(3～5)mL。
作为上述工艺的优选，步骤(2)中，微波辅助提取的温度为100～120℃。
作为上述工艺的优选，步骤(2)中，微波辅助提取的时长为25～45min。
作为上述工艺的优选，步骤(2)中，微波辅助提取的功率为600～800W。
作为上述工艺的优选，步骤(3)中，加热水提的温度为50～80℃，水提2～3次。
作为上述工艺的优选，步骤(3)中，加热水提前，将剩余物置于-5℃～0℃下处理2～4h。
作为上述工艺的优选，：步骤(4)中，水提液A用体积百分比为95～100％的乙醇溶液醇沉。
作为上述工艺的优选，步骤(4)中，水提液A还可以依次用体积百分比为30～50％的乙醇溶液、体积百分比为60～80％的乙醇溶液、体积百分比为95～100％的乙醇溶液，醇沉3次，合并3次醇沉沉淀作为沉淀物C，上清液为水提液B。
本发明的有益效果是：
本发明工艺采用微波辅助提取工艺提取生姜精油，并对生姜精油提取后剩余物进一步提取活性物质，通过加热水提、醇沉等技术，进一步获得生姜不溶性膳食纤维粗提物、生姜抗氧化剂和生姜多糖。本发明工艺综合提取的四种活性物质得率理想，并且不含有毒有害溶剂，符合食品原料要求，可用于高附加值产品的开发生产，将生姜精油提取后的剩余物回收利用，不仅能增加生产企业的经济效益，还可减轻废弃物排放造成的环境污染，其市场前景广阔且具有重大的社会意义。
具体实施方式
实施例1
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入150mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率800W，提取25min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例2
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入250mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率600W，提取45min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例3
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入200mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率700W，提取35min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例4
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，加入乙醇，乙醇的添加量为生姜重量的5％，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入250mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率800W，提取45min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例5
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，加入乙醇，乙醇的添加量为生姜重量的10％，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入200mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率700W，提取35min，分离获得生姜精油，将剩余物在-4℃下处理3h，再加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例6
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，加入乙醇，乙醇的添加量为生姜重量的2％，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入200mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率700W，提取35min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A依次用体积百分比为30～50％的乙醇溶液、体积百分比为60～80％的乙醇溶液、体积百分比为95～100％的乙醇溶液，醇沉3次，水提液A与每次醇沉的乙醇溶液的体积比为1：4，合并3次醇沉沉淀作为沉淀物C，上清液为水提液B，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例7
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，加入乙醇，乙醇的添加量为生姜重量的5％，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入250mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率800W，提取45min，分离获得生姜精油，将剩余物在-4℃下处理3h，再加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A依次用体积百分比为30～50％的乙醇溶液、体积百分比为60～80％的乙醇溶液、体积百分比为95～100％的乙醇溶液，醇沉3次，水提液A与每次醇沉的乙醇溶液的体积比为1：4，合并3次醇沉沉淀作为沉淀物C，上清液为水提液B，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例8
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入100mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率500W，提取25min，分离获得生姜精油，将剩余物加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A依次用体积百分比为30～50％的乙醇溶液、体积百分比为60～80％的乙醇溶液、体积百分比为95～100％的乙醇溶液，醇沉3次，水提液A与每次醇沉的乙醇溶液的体积比为1：4，合并3次醇沉沉淀作为沉淀物C，上清液为水提液B，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例9
一种生姜中活性物质的综合提取工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL圆底烧瓶中，加入50mL水混合，置在微波萃取仪中，用微波辅助提取，设定微波温度100℃，微波功率600W，提取50min，分离获得生姜精油，将剩余物在-4℃下处理3h，再加热至60℃，水提2次，置于离心机上，4200g离心40min，获得水提液A和残渣，将残渣用烘箱50℃烘干，获得生姜不溶性膳食纤维粗提物；水提液A用纯乙醇沉淀，水提液A与纯乙醇的体积比为1：4，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
实施例1～9工艺提取的各产物得率
生姜精油成分分析
利用GC-MS法分析实施例7的生姜精油成分，能够从生姜精油中有效地分离到109种化合物，进一步定量分析发现，姜精油以异戊二烯结构的萜烯类(碳氢类)化合物为主，同时含有醇类、酮类、醛类等组分；单组分含量最高的是姜烯(24.18％)，其次是桧烯(11.02％)、β-柠檬醛(9.42％)、β-倍半水芹烯(7.20％)、α-柠檬醛(5.92％)、α-金合欢烯(5.74％)、莰烯(5.32％)。
生姜抗氧化剂的成分分析
高效液相色谱-电喷雾质谱法(HPLC-ESI-MS/MS)测定了生姜抗氧化剂提取物的成分，其中4种成分被识别；柠檬酸(653.7μg/g)、咖啡酸(3.9μg/g)、对香豆酸(109.6μg/g)、阿魏酸(75.8μg/g)。
对比例
采用常规溶剂辅助提取蒸馏工艺，将生姜表面的污物清洗干净，切成均匀的块状，用高速搅拌机将其搅成泥状，取250g泥状生姜，置于500mL蒸馏烧瓶中，加入150mL体积百分比为30％的乙醇，混合，蒸馏3h，分离获得生姜精油。
生姜精油得率0.207g/100g生姜鲜重。
Claims (10)
1.一种生姜中活性物质的综合提取工艺，包括如下制备步骤：
(1)将新鲜的生姜清洗干净，切块，搅成泥状；
(2)将步骤(1)获得的泥状生姜与水混合，用微波辅助提取，分离，获得生姜精油和剩余物；
(3)将剩余物加热水提，离心，获得水提液A和残渣，将残渣干燥，获得生姜不溶性膳食纤维粗提物；
(4)水提液A用乙醇醇沉，获得水提液B和沉淀物C，水提液B经蒸干后获得生姜抗氧化剂；沉淀物C为生姜多糖。
2.根据权利要求1所述的综合提取工艺，其特征在于：步骤(1)中，切块后加入乙醇，乙醇的添加量为生姜重量的1～10％。
3.根据权利要求1所述的综合提取工艺，其特征在于：步骤(2)中，泥状生姜与水按质量体积比为5g：(3～5)mL。
4.根据权利要求1所述的综合提取工艺，其特征在于：步骤(2)中，微波辅助提取的温度为100～120℃。
5.根据权利要求1所述的综合提取工艺，其特征在于：步骤(2)中，微波辅助提取的时长为25～45min。
6.根据权利要求1所述的综合提取工艺，其特征在于：步骤(2)中，微波辅助提取的功率为600～800W。
7.根据权利要求1所述的综合提取工艺，其特征在于：步骤(3)中，加热水提的温度为50～80℃，水提2～3次。
8.根据权利要求1所述的综合提取工艺，其特征在于：步骤(3)中，加热水提前，将剩余物置于-5℃～0℃下处理2～4h。
9.根据权利要求1所述的综合提取工艺，其特征在于：步骤(4)中，水提液A用体积百分比为95～100％的乙醇溶液醇沉。
10.根据权利要求1所述的综合提取工艺，其特征在于：步骤(4)中，水提液A还可以依次用体积百分比为30～50％的乙醇溶液、体积百分比为60～80％的乙醇溶液、体积百分比为95～100％的乙醇溶液，醇沉3次，合并3次醇沉沉淀作为沉淀物C，上清液为水提液B。
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