CN103598544B - 以大蒜为原料进行综合利用的提取工艺 - Google Patents
以大蒜为原料进行综合利用的提取工艺 Download PDFInfo
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Abstract
本发明公开了一种以大蒜为原料进行综合利用的提取工艺。该工艺是将大蒜打磨成浆液进行固、液分离,固体物经干燥得无臭蒜粉;液相通过强酸型阳离子吸附蒜氨酸,流出液则为大蒜多糖溶液,溶液经浓缩、干燥得大蒜多糖粉;吸附蒜氨酸的树脂用0.5mol/L氨水溶液进行洗脱,收集洗脱液经浓缩、干燥得蒜氨酸产品。再将上述无臭蒜粉进行水解、离心分离去除上清液得大蒜蛋白,经干燥后得大蒜蛋白粉;将大蒜蛋白粉进行一次、二次酶解,分离后得上清液和沉淀物;分别将上清液进行第三次酶解、灭酶、浓缩、干燥得大蒜糖肽;将沉淀物进行第三次酶解、灭酶经分离取上清液和沉淀物分别进行干燥后得氨基酸平衡肽和大蒜多肽。该工艺综合利用效率高,工艺路线合理。
Description
技术领域
本发明涉及以大蒜为原料综合提取有效成分的深加工工艺,具体涉及一种以大蒜为原料进行综合利用的提取工艺。
背景技术
大蒜是百合科葱属植物蒜(Allium Satiuum L.)的地下鳞茎,大蒜自古以来是作为蔬菜和调味品,但作为药用原料使用也有5000年的历史,药用价值在古代埃及、印度、中国都有记载。中医理论认为,大蒜味辛性温,有行气滞、暖脾胃、解毒、杀虫等独到功效。目前国内外的科学家对大蒜的研究都相当重视,从药理、临床、应用等各个方面进行了系统深入的研究,取得了大量的科研成果,进一步证明了大蒜不仅是一种良好的保健食品,也是一种具有广泛应用前景的天然药品。特别是大蒜富含的有效生物活性成分和营养物质成分被有效地提取应用后,给大蒜这一传统产品带来了更多有用的价值。大蒜的化学成分比较复杂,包括常规营养成分如氨基酸、维生素、碳水化合物以及大蒜油等。100g鲜大蒜含水70g、蛋白质4.4g、脂肪0.2g、碳水化合物23g、粗纤维0.7g、灰分1.3g,其中钙5mg、磷44mg、铁0.4g、维生素D0.24mg、维生素B20.03mg、烟酸0.9mg、维生素C3mg、大蒜油0.2g。大蒜中含有17种氨基酸,其中以赖氨酸、亮氨酸、缬氨酸的含量较高。富含的维生素有维生素C、B1、B2、P和维生素A等,其中维生素C含量为最高。大蒜中的酶除蒜氨酸酶外,还含有水解酶、聚果糖苷酶、反果糖苷酶、转化酶、过氧化酶等。大蒜中的碳水化合物有还原糖(以葡萄糖和果糖为主)、蔗糖、多聚糖等。从各种碳水化合物所占比例来看,以多聚糖最高,达到51%,其次为淀粉8.22%,糊精7.69%,蔗糖3.79%,还原糖0.14%。现有研究报导最多是针对大蒜中主要活性成分,如大蒜素(油)大蒜氨基酸(蒜氨酸)、大蒜多糖,且均有不同的提取方法制得产品供应市场,然而这些单一的提取方法是将大蒜中的其他物质均作为废弃物丢弃的。就大蒜中的蛋白质等营养成分均未得到充分利用,这给资源造成了浪费,将大蒜蛋白质进行有效地提取,再经水解生产肽类产品是综合利用大蒜的一种重要手段,由于小分子肽具有独特的生理活性和许多特殊的营养功能以及生理活性,在医学界和营养学界颇受关注。大蒜蛋白是一种糖蛋白,然而糖蛋白是蛋白质和带有分支的寡链糖相连形成的共价复合物,它是生物体的重要组成部分,在生物体的生命活动中起到重要的作用,有诸如细胞信号识别、生长调控、细胞间信息传递及免疫调节等生理功能,这些特点说明糖肽较一般的肽更有生理活性。充分利用大蒜蛋白质是综合利用大蒜的有价值的方法。目前国内就利用大蒜为原料制备各种大蒜蛋白肽的工艺技术尚未见有报道。而以大蒜为原料进行综合利用的提取工艺也尚未见有报道。
发明内容
本发明的目的是为了提供一种以大蒜为原料通过打浆、分离、酶解等工艺,获得了对大蒜进行深加工的工艺。
一种以大蒜为原料进行综合利用的提取工艺,其特征在于包括以下工艺步骤:
步骤(一) 将大蒜用清水反复漂洗3次以上,以除去杂质,剥开蒜瓣,置入35-45℃的温水中浸泡2小时,搓出蒜瓣,并去除带斑、伤疤、干瘪、病污的杂瓣蒜,漂洗干净后,置于含有重量比为6%的食盐沸水中,烫漂3-6分钟进行钝化处理;目的是钝化蒜氨酸酶,抑制大蒜臭味产生,软化组织,破碎更方便;
步骤(二) 将钝化后的蒜瓣,先置入砂轮磨中加入蒜瓣重量2-10倍的纯净水进行粗磨后,再迅即送入胶体磨中进行细磨15-20分钟,使成均匀的乳状浆液后,置入不锈钢夹层锅中,隔层加热45-85℃,搅拌提取30-120分钟后,经离心分离得溶液和沉淀物;
步骤(三) 将步骤(二)分离得到的沉淀物经40-55℃真空干燥、粉碎得无臭蒜粉;
步骤(四) 将步骤(二)分离得到的溶液,在35-45℃条件下,快速搅拌加入体积量30%的含有重量比为0.25-10%的吸附澄清剂溶液,恒温在35-40℃保温1小时,然后置于0-4℃冷藏24小时,离心分离,得澄清液,将清液通过H+型001×7强酸性阳离子交换树脂交换,流速为1-5倍床体积/h进行吸附蒜氨酸,流出液为大蒜多糖溶液;
步骤(五) 将步骤(四)得到的大蒜多糖溶液,采用薄膜蒸发浓缩至溶液体积的1/3,然后进行喷雾干燥得大蒜多糖粉;为了改善大蒜多糖粉的品质和口感,还可以加入大蒜多糖溶液总重量2-10%的添加剂。
其中所述的添加剂是β-环糊精、麦芽糊精、海藻酸钠、蔗糖、果糖、山梨糖醇、葡萄糖、木糖醇、L-阿拉伯糖、β-葡聚糖中的任意一种。
步骤(六) 将步骤(四)吸附蒜氨酸后的树脂用纯净水冲洗干净后,用0.5mol/L氨水溶液进行洗脱,收集洗脱液,减压浓缩至洗脱液体积在1/5-1/10,得浓缩液,采用0.22μm微孔滤膜过滤,滤液中加入医用级乙醇至溶液体积乙醇含量为50-80%,调节PH值5.0-7.0,置于0-4℃冷藏24-40小时后,分离得蒜氨酸,经38-48℃低温真空干燥,得蒜氨酸产品;
步骤(七) 将步骤(三)获得的无臭蒜粉按重量比加入20-40倍的纯净水,充分搅匀,加热35-65℃,用1mol/L氢氧化钠溶液调节PH值至6.8-10之间进行溶解,在不断搅拌下,浸泡2小时,然后静置1小时后,再用0.5mol/L盐酸调节PH值3.9-4.9之间,加热煮沸1.5小时,然后静置沉淀,离心除去上清液,得沉淀物,再将沉淀物按重量比加入10倍量的纯净水,搅匀后静置30分钟,离心甩干水分得大蒜蛋白,经干燥后得大蒜蛋白粉;
步骤(八) 将步骤(七)得到的大蒜蛋白粉,溶解进行第一次酶解,溶解条件为大蒜蛋白在水中的重量浓度为2.5-10%、温度为30-65℃、PH值为6.6-7.2之间进行溶解后,先用中性蛋白酶进行酶解,其中条件为中性蛋白酶的重量为大蒜蛋白溶液重量的1-3%、控制PH值为6.5-6.9、保温45-55℃、酶解时间为3-4.5小时,得中性蛋白酶酶解液,然后将酶解液再加入复合风味蛋白酶进行二次酶解,其中条件为:复合风味蛋白酶的重量为大蒜蛋白溶液重量的1.0-2.5%,PH值自然(不需调整)、保温49-52℃、酶解时间为4-7.5小时,得酶解液,然后将酶解液用1mol/L盐酸调节PH值在4.2-4.4之间,静置沉淀使自然冷却后,进行离心分离得上清液和沉淀物;
步骤(九) 将步骤(八)得到的上清液用复混(配)蛋白酶进行第三次酶解,然后加热至98℃灭酶,经浓缩、喷雾干燥得大蒜糖肽;将步骤(八)得到的沉淀物用复混蛋白酶进行第三次酶解,然后加热至98℃灭酶,经离心分离取上清液,经浓缩、喷雾干燥得氨基酸平衡肽;取沉淀进行真空干燥得大蒜多肽。
所述步骤(九)中的上清液酶解条件是PH值为6.5-7.0、温度46-52℃,酶解时间为5.5-7.5小时,酶解时,复混蛋白酶的重量为上清液重量的1.6-2.8%。
所述步骤(九)中的沉淀物酶解时的投料重量浓度为1.5-2.0%;其中酶解条件是温度为48-52℃、酶解时间为7-8.5小时;酶解时,复混蛋白酶的重量为沉淀物溶解液重量的0.9-1.8%。
所述步骤(九)中的复混蛋白酶,是由中性蛋白酶与复合风味蛋白酶按重量份1:2复配混合制得。
所述步骤(四)中的吸附澄清剂溶液为硅藻土、明胶、海藻酸钠、壳聚糖、101果汁澄清剂(郑州天顺食品添加剂有限公司出品)、ZTC1+1天然澄清剂(北京正天成澄清技术有限公司出品)中的任意一种,经公知工艺制备成0.25-10%的溶液。
所述的大蒜多糖、蒜氨酸、大蒜糖肽、氨基酸平衡肽、大蒜多肽产品,分别由权利要求1所述的方法获得。
中性蛋白酶(SUKAPRO NE):蛋白酶Neutrase是由淀粉液化芽孢杆菌族生产的内蛋白酶制剂,被广泛用于动、植物的蛋白质加工业,以改变蛋白质的水结合能力、乳化能力、发泡能力及其粘度,能将蛋白质水解为低分子蛋白胨、月示 、多肽及氨基酸,中性蛋白酶由中性蛋白酶高产菌株--杆菌(BacuiLLus)深层发酵而成,在中性条件下具有较高的活性,能在中性条件下水解植物蛋白质中的缩氨酸键,释放氨基酸或者多肽,中性蛋白酶适用PH范围是6.0-8.0,最适PH值6.8-7.0,温度范围是10℃-60℃,最适温度45-50℃,然而根据本发明对比试验结果表明,结果显示在温度为48-52℃、PH值为6.6-6.8时酶解效果最佳,其发酵液的澄清度最好。
复合风味蛋白酶(Flavourzyme)是由米曲霉生产的内蛋白酶和外蛋白酶混合制剂(内蛋白酶为切割多肽键内部的肽键;外蛋白酶则为切割多肽链一端的肽键)再外加一些风味物质复配而成的复合风味蛋白酶,其特点是酶解后期风味优化,去除苦味,改善口感,可以制取风味良好的水解产品,提高产品质量,本产品含有氨肽酶,羧肽酶,通过末端水解多肽,可提高水解度。复合风味蛋白酶最适PH值是6.0-7.0,温度50-53℃,其酶解条件与中性蛋白酶基本相似。
本发明比现有技术具有如下优点:
1.本发明采用大蒜为基本原料,通过对蒜瓣的组织分离,离子交换、酶解等工艺对大蒜的有益成分进行综合提取,分别获得大蒜多糖、蒜氨酸、大蒜蛋白粉、氨基酸平衡肽和大蒜多肽产品。
2.本发明采取一次性投料连续提取的综合工艺,突破了大蒜成分单一提取的模式,使得大蒜原料能够得到充分利用,节约了资源,降低了加工成本,减少了大蒜常规加工提取造成的资源浪费,提高了生产效率,提升了大蒜原料的利用率,提高了经济效益,提升了大蒜综合利用的竞争力。
3.本发明的综合提取工艺技术成熟、工艺独特,综合利用效率高,成本低廉,产品安全、无毒副作用,一次性投料达到多步连续提取制得的不同产品,均具有营养和辅助的保健功效,可广泛应用于医药、药用辅料,保健食品和食品添加剂。
4.本发明制备工艺具有工艺简单和方便的操作性及实用性,工艺路线明确,生产安全,无污染,环保清洁、卫生,适宜工业化规模性生产。大蒜综合提取工艺的实施具有很好经济价值和经济效益。
具体实施方式
结合以下实施例针对本发明作进一步说明,而非是本发明的限制。
实施例1
将大蒜用清水反复漂洗3次以上,除去杂质,剥开蒜瓣,置入35-45℃的热水中浸泡2小时后,搓出蒜瓣,挑除带斑、伤疤、干瘪、病污的杂瓣蒜,进行漂洗干净,置入含有重量比为6%的食盐沸水中,烫漂3-6分钟进行钝化处理,得钝化蒜瓣。
实施例2
将实施例1经钝化处理后的蒜瓣按重量比加入2-10倍的纯净水,置入砂轮磨中进行粗磨后,再迅即送入胶体磨中进行细磨15-20分钟,使成均匀的乳状浆液,置入不锈钢夹层锅中,隔层蒸汽加热45-85℃,搅拌提取30-120分钟后,经离心分离得溶液和沉淀物,将分离得到的沉淀物经40-55℃真空干燥、粉碎得无臭蒜粉。
实施例3
将实施例2经离心分离得到的溶液,在35-45℃条件下,快速搅拌加入溶液体积30%的用重量比2.5%的醋酸液配成含有重量比为1%壳聚糖澄清剂溶液,控温35-40℃、保温1小时,然后置于0-4℃冷藏24小时,离心分离,得澄清液,再将澄清液通过H+型001×7强酸性阳离子交换树脂交换;控制流速为1bv/h进行吸附蒜氨酸,流出液为大蒜多糖溶液;
实施例4
将实施例3经离子交换树脂交换后的大蒜多糖溶液,采用薄膜蒸发浓缩至溶液体积的1/3,然后进行喷雾干燥得大蒜多糖粉。
实施例5
将实施例3经离子交换树脂交换后的大蒜多糖液,加热40-50℃,在不断搅拌下加溶液重量比2.5%的β-环糊精,使溶解后,继续搅拌30分钟后,经薄膜蒸发浓缩至溶液体积的1/3,然后进行喷雾干燥得大蒜多糖粉。
实施例6
将实施例3吸附蒜氨酸后的树脂用纯净水冲洗干净,用0.5moL/L氨水溶液进行洗脱,收集洗脱液,减压浓缩至洗脱液体积在1/5时得浓缩液,用0.22μm微孔滤膜过滤,滤液中加入医用级乙醇至溶液体积乙醇含量为50-80%,调整PH值5.0-7.0,置于0-4℃环境下冷藏24-40小时,分离得蒜氨酸湿品,经38-48℃低温真空干燥,得蒜氨酸产品。
实施例7
将实施例2得到的无臭蒜粉按重量比加入20-40倍的纯净水,充分搅匀,加热35-65℃,用1moL/L氢氧化钠溶液调节PH值至6.8-10之间进行溶解,在不断搅拌下,浸泡2小时,然后静置1小时后,再用0.5moL/L盐酸调节PH值至3.9-4.9之间,加热煮沸1.5小时,然后静置沉淀,离心分离除去上清液,得沉淀物,再将沉淀物按重量比加入10倍量的纯净水,搅匀后静置30分钟,离心甩干水分得大蒜蛋白,经干燥后得大蒜蛋白粉。
实施例8
将实施例7得到的大蒜蛋白粉加纯净水,使成大蒜蛋白在水中的重量浓度为2.5-10%、加热至30-65℃,调节PH值为6.6-7.2之间进行溶解后,加入大蒜蛋白溶液重量的1-3%的中性蛋白酶进行第一次酶解,酶解条件是控制PH为6.5-6.9,保温45-55℃、酶解时间为3-4.5小时,然后将中性蛋白酶解液再加入复合风味蛋白酶进行二次酶解,其条件是复合风味蛋白酶的重量为大蒜蛋白溶液重量的1.0-2.5%,PH值自然,保温49-52℃,酶解时间为4-7.5小时,得酶解液,然后将酶解液用1moL/L盐酸调节PH值在4.2-4.4之间,静置沉淀使自然冷却后,进行离心分离得上清液和沉淀物;将上清液加入复混蛋白酶的重量为上清液重量的1.6-2.8%进行第三次酶解,第三次酶解控制PH值为6.5-7.0、温度46-52℃,时间为5.5-7.5小时,然后98℃灭酶,经浓缩、喷雾干燥得大蒜糖肽。
实施例9
将实施例8经二次酶解后分离得到的沉淀物加纯净水配成质量浓度为1.5-2.0%,加入复混蛋白酶的重量为沉淀物溶解液重量的0.9-1.8%,在温度为48-52℃条件下,酶解7-8.5小时,然后加热98℃灭酶,离心分离取上清液,经浓缩、喷雾干燥得氨基酸平衡肽。取沉淀进行真空干燥得大蒜多肽。
以上实施例中的复混蛋白酶,是由中性蛋白酶与复合风味蛋白酶按重量份1:2复配混合制得。
Claims (8)
1. 一种以大蒜为原料进行综合利用的提取工艺,其特征在于,包括以下工艺步骤:
步骤(一) 将大蒜用清水反复漂洗3次以上,以除去杂质,剥开蒜瓣,置入35-45℃的温水中浸泡2小时,搓出蒜瓣,并去除带斑、伤疤、干瘪、病污的杂瓣蒜,漂洗干净后,置于含有重量比为6%的食盐沸水中,烫漂3-6分钟进行钝化处理;
步骤(二) 将钝化后的蒜瓣,先置入砂轮磨中加入蒜瓣重量2-10倍的纯净水进行粗磨后,再迅即送入胶体磨中进行细磨15-20分钟,使成均匀的乳状浆液后,置入不锈钢夹层锅中,隔层加热45-85℃,搅拌提取30-120分钟后,经离心分离得溶液和沉淀物;
步骤(三) 将步骤(二)分离得到的沉淀物经40-55℃真空干燥、粉碎得无臭蒜粉;
步骤(四) 将步骤(二)分离得到的溶液,在35-45℃条件下,快速搅拌加入体积量30%的含有重量比为0.25-10%的吸附澄清剂溶液,恒温在35-40℃保温1小时,然后置于0-4℃冷藏24小时,离心分离,得澄清液,将清液通过H+型001×7强酸性阳离子交换树脂交换,流速为1-5倍床体积/h进行吸附蒜氨酸,流出液为大蒜多糖溶液;
步骤(五) 将步骤(四)得到的大蒜多糖溶液,采用薄膜蒸发浓缩至溶液体积的1/3,然后进行喷雾干燥得大蒜多糖粉;
步骤(六) 将步骤(四)吸附蒜氨酸后的树脂用纯净水冲洗干净后,用0.5mol/L氨水溶液进行洗脱,收集洗脱液,减压浓缩至洗脱液体积在1/5-1/10,得浓缩液,采用0.22μm微孔滤膜过滤,滤液中加入医用级乙醇至溶液体积乙醇含量为50-80%,调节pH值5.0-7.0,置于0-4℃冷藏24-40小时后,分离得蒜氨酸,经38-48℃低温真空干燥,得蒜氨酸产品;
步骤(七) 将步骤(三)获得的无臭蒜粉按重量比加入20-40倍的纯净水,充分搅匀,加热35-65℃,用1mol/L氢氧化钠溶液调节pH值至6.8-10之间进行溶解,在不断搅拌下,浸泡2小时,然后静置1小时后,再用0.5mol/L盐酸调节pH值3.9-4.9之间,加热煮沸1.5小时,然后静置沉淀,离心除去上清液,得沉淀物,再将沉淀物按重量比加入10倍量的纯净水,搅匀后静置30分钟,离心甩干水分得大蒜蛋白,经干燥后得大蒜蛋白粉;
步骤(八) 将步骤(七)得到的大蒜蛋白粉,溶解进行第一次酶解,溶解条件为大蒜蛋白在水中的重量浓度为2.5-10%、温度为30-65℃、pH值为6.6-7.2之间进行溶解后,先用中性蛋白酶进行酶解,其中条件为中性蛋白酶的重量为大蒜蛋白溶液重量的1-3%、控制pH值为6.5-6.9、保温45-55℃、酶解时间为3-4.5小时,得中性蛋白酶酶解液,然后将酶解液再加入复合风味蛋白酶进行二次酶解,其中条件为:复合风味蛋白酶的重量为大蒜蛋白溶液重量的1.0-2.5%,pH值不需调整、保温49-52℃、酶解时间为4-7.5小时,得酶解液,然后将酶解液用1mol/L盐酸调节pH值在4.2-4.4之间,静置沉淀使自然冷却后,进行离心分离得上清液和沉淀物;
步骤(九) 将步骤(八)得到的上清液用复混蛋白酶进行第三次酶解,然后加热至98℃灭酶,经浓缩、喷雾干燥得大蒜糖肽;将步骤(八)得到的沉淀物用复混蛋白酶进行第三次酶解,然后加热至98℃灭酶,经离心分离取上清液,经浓缩、喷雾干燥得氨基酸平衡肽;取沉淀进行真空干燥得大蒜多肽。
2. 如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,其特征在于所述步骤(四)中的吸附澄清剂溶液为硅藻土、明胶、海藻酸钠、壳聚糖、101果汁澄清剂、ZTC1+1天然澄清剂中的任意一种,经公知工艺制备成0.25-10%的溶液。
3. 如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,其特征在于所述步骤(五)中大蒜多糖粉包括大蒜多糖溶液总重量2-10%的添加剂。
4. 根据权利要求3所述的以大蒜为原料进行综合利用的提取工艺,其特征在于,所述的添加剂是β-环糊精、麦芽糊精、海藻酸钠、蔗糖、果糖、山梨糖醇、葡萄糖、木糖醇、L-阿拉伯糖、β-葡聚糖中的任意一种。
5. 如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,其特征在于所述步骤(九)中的上清液酶解条件是pH值为6.5-7.0、温度46-52℃,酶解时间为5.5-7.5小时,酶解时,复混蛋白酶的重量为上清液重量的1.6-2.8%。
6. 如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,其特征在于所述步骤(九)中的沉淀物酶解时的投料重量浓度为1.5-2.0%;其中酶解条件是温度为48-52℃、酶解时间为7-8.5小时;酶解时,复混蛋白酶的重量为沉淀物溶解液重量的0.9-1.8%。
7. 如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,其特征在于所述步骤(九)中的复混蛋白酶,是由中性蛋白酶与复合风味蛋白酶按重量份1:2复配混合制得。
8. 一种如权利要求1所述的以大蒜为原料进行综合利用的提取工艺,分别获得大蒜多糖、蒜氨酸、大蒜糖肽、氨基酸平衡肽、大蒜多肽产品。
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