CN115486530B - 一种迷迭香的冷冻干燥方法 - Google Patents
一种迷迭香的冷冻干燥方法 Download PDFInfo
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- CN115486530B CN115486530B CN202211292833.0A CN202211292833A CN115486530B CN 115486530 B CN115486530 B CN 115486530B CN 202211292833 A CN202211292833 A CN 202211292833A CN 115486530 B CN115486530 B CN 115486530B
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Abstract
本发明属于天然植物成分深加工领域,公开了一种迷迭香的冷冻干燥方法,包括以下步骤:1)迷迭香的采收、2)迷迭香的保鲜清洗、3)初步自然干燥、4)迷迭香粉碎、5)烘干干燥、6)预冻、7)冷冻干燥,本发明所述的冷冻干燥方法中,调整了制备工艺,相比现有技术,添加了自研的保鲜清洗液和冻干保护剂,能够最大限度的保留迷迭香的天然有效成分,进一步的,本发明还改进了从上述迷迭香中提取迷迭香精油的提取液成分;本发明所述的方法相比现有技术,有机溶剂的使用量大大减少,最终产品中几乎没有乙醇残留,同时冻干流程短,节能减排,降低成本效果显著。
Description
技术领域
本发明属于天然植物成分深加工领域,公开了一种迷迭香的冷冻干燥方法。
背景技术
迷迭香,拉丁学名(Rosmarinusofficinalis),是双子叶植物纲、唇形科、迷迭香属植物灌木。性喜温暖气候,原产欧洲地区和非洲北部地中海沿岸。远在曹魏时期就曾引种中国。园林中偶有应用。从迷迭香的花和叶子中能提取具有优良抗氧化性的抗氧化剂和迷迭香精油。迷迭香抗氧化剂。广泛用于医药、油炸食品、富油食品及各类油脂的保鲜保质;而迷迭香香精则用于香料、空气清新剂、驱蚁剂以及杀菌、杀虫等日用化工业。
迷迭香具有镇静提神、醒脑作用,对消化不良和胃痛均有一定疗效。多将其捣碎后,用开水浸泡后饮用,1天2~3次,可起到镇静、利尿作用。也可用于治疗失眠、心悸、头痛、消化不良等多种疾病。外用可治疗外伤和关节炎。还具有强壮心脏、促进代谢、促进末梢血管的血液循环等作用。在西餐中迷迭香是经常使用的香料,在牛排、土豆等料理以及烤制品中特别经常使用。清甜带松木香的气味和风味,香味浓郁,甜中带有苦味。
为了方便迷迭香运输和进一步的加工,需要对采收的迷迭香进行干燥并进行有效成分的提取,目前工业化中,对迷迭香的干燥主要有自然晾干,加热烘干以及冷冻干燥;冷冻干燥法由于能够最大程度的保留迷迭香之中的迷迭香抗氧化剂和精油,并且方便长期保存和运输,因此越来越普及,例如CN201410204635.3公开了一种迷迭香复配提取物的制备方法,提到的冷冻干燥方法如下:(1)取新鲜的迷迭香叶茎,将迷迭香叶茎展开,在温度为-6~-9℃的环境下进行冷冻,冷冻时间为6h~10h;(2)从冷冻室中取出迷迭香叶茎,将迷迭香叶茎真空冷冻干燥,真空冷冻干燥的压强为11Pa~17Pa,冷冻干燥时间为5h~7h;(3)将迷迭香叶茎从冷冻干燥机中取出,粉碎迷迭香叶茎,粉碎至叶茎粉为200~300目,放置在干燥环境中。(4)取迷迭香叶茎粉末,将迷迭香叶茎粉末用乙醇进行搅拌提取。上述发明的工艺过程中,迷迭香乙醇提取率最高仅为20%,造成对原料的巨大浪费,同时需要消耗大量的有机溶剂,乙醇残留量高,不够绿色环保。因此需要寻找一种绿色环保高效的迷迭香冷冻干燥以及提取的工艺。
发明内容
为了解决上述问题,本发明公开了一种迷迭香的冷冻干燥方法。
本发明的技术方案如下:
一种迷迭香的冷冻干燥方法,其特征在于,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-45~-55℃,压强300-800Pa,冻干30-60min;
B:-60~-55℃,压强150-250Pa,冻干100-200min;
C:-75~-85℃,压强70-150Pa,冻干30-45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装。
本方案中,采用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗,洗去迷迭香嫩叶上的灰尘,泥土,并对嫩叶进行保鲜,防止有效成分散失,同时对迷迭香嫩叶进行杀菌,去除农药残留;同时先对迷迭香进行自然干燥和烘干干燥,使得含水量低于15%,而不是马上进行冻干,是为了降低水分,从而降低冻干的时间和能耗,随后在冻干时加入冻干保护剂,进一步的降低迷迭香在冻干时有效成分的破坏,并使用程序的冻干,保证冻干质量的同时降低冻干的总时间。
进一步的,上述一种迷迭香的冷冻干燥方法,所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。上述范围内的新鲜嫩叶一般来说处于韧皮部和木质部的分界线之上,质量最好,迷迭香有效成分含量最多。
进一步的,上述一种迷迭香的冷冻干燥方法,所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
采用上述保鲜清洗液,可以洗去迷迭香嫩叶上的灰尘,泥土,并对嫩叶进行保鲜,防止有效成分散失,同时对迷迭香嫩叶进行杀菌,去除农药残留。葡萄糖酸氯己定是一种双胍氯苯,有相当广的抗微生物活性,十二烷基硫酸钠具有强力的去污能力,并能够直接洗去农药残留,同时L-半胱氨酸具有很好的解毒中和生物中和能力,能够与无法洗去的农药残留中和,与十二烷基硫酸钠配合使用能够彻底去除农药残留影响;L-抗坏血酸具有强大的抗氧化作用,能够防止迷迭香的氧化变质有效成分丧失。
进一步的,上述一种迷迭香的冷冻干燥方法,所述步骤2)中的浸泡时间为2-6h,温度为15-30℃。浸泡时间过短无法实现灰尘和农药残留的洗涤,时间太长容易腐败,经过实验发现2-6小时比较容易实现上述的平衡。
进一步的,上述一种迷迭香的冷冻干燥方法,所述步骤7)中的冻干保护剂选自甘油,阿拉伯胶或海藻糖中的一种。
进一步的,上述一种迷迭香的冷冻干燥方法,所述海藻糖经过如下步骤的改性:
a.称取海藻糖原料投入含有质量分数为1-3%氢氧化钠溶液中超声波清洗10-20min,随后放入质量分数0.5-1%的冰醋酸溶液中,对海藻糖溶液进行抽滤,然后用95%以上乙醇沉淀洗涤,干燥获得预处理海藻糖;
b.将预处理海藻糖与质量分数5-10%醋酸溶液加入反应容器,所述海藻糖原料与所述醋酸溶液的质量体积比为1g:5-10mL;冰水浴控制反应温度在0~5℃;在搅拌的状态下加入羟化卵磷脂;滴加完毕后撤去冰水浴,在室温下持续搅拌反应2~4h;经静置、沉淀、抽滤、干燥、重结晶得到改性海藻糖;其中所述预处理壳聚糖与羟化卵磷脂的质量比为1:(0.3~0.5)。
经过申请人实验发现,使用上述改性的海藻糖,对于迷迭香的冻干保护力最强。
进一步的,上述一种迷迭香的冷冻干燥方法制备获得的迷迭香。
进一步的,一种迷迭香有效成分的提取工艺,包含上述冷冻干燥方法。
进一步的,上述迷迭香有效成分的提取工艺,其特征在于,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-45~-55℃,压强300-800Pa,冻干30-60min;
B:-60~-55℃,压强150-250Pa,冻干100-200min;
C:-75~-85℃,压强70-150Pa,冻干30-45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:5-10的比例投入提取液中4-10℃浸泡12-24h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 10-20份
L-抗坏血酸 0.5-1份;
随后将含有迷迭香冻干粉提取液进行蒸馏提取获得迷迭香精油。
本方案中,使用低毒对环境无害的丙三醇作为提取液主要成分,配合L-抗坏血酸对迷迭香冻干粉进行浸出,绿色环保,同时能够最大程度保留有效活性成分。
进一步的,经过上述迷迭香有效成分的提取工艺制备得到的迷迭香精油。
相比现有技术,本发明具有如下有益效果:
1)本发明公开了一种迷迭香的冷冻干燥方法,从采摘开始就注重最大程度保留迷迭香的有效成分,选择从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。上述范围内的新鲜嫩叶一般来说处于韧皮部和木质部的分界线之上,质量最好,迷迭香有效成分含量最多。整个工艺中,采用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗,洗去迷迭香嫩叶上的灰尘,泥土,并对嫩叶进行保鲜,防止有效成分散失,同时对迷迭香嫩叶进行杀菌,去除农药残留;同时先对迷迭香进行自然干燥和烘干干燥,使得含水量低于15%,而不是马上进行冻干,是为了降低水分,从而降低冻干的时间和能耗,随后在冻干时加入冻干保护剂,进一步的降低迷迭香在冻干时有效成分的破坏,并使用程序的冻干,保证冻干质量的同时降低冻干的总时间,相比普通的冻干程序,能够节省一半或者三分之二的时间。
2)本发明还配制了一种保鲜清洗液,采用上述保鲜清洗液,可以洗去迷迭香嫩叶上的灰尘,泥土,并对嫩叶进行保鲜,防止有效成分散失,同时对迷迭香嫩叶进行杀菌,去除农药残留。葡萄糖酸氯己定是一种双胍氯苯,有相当广的抗微生物活性,十二烷基硫酸钠具有强力的去污能力,并能够直接洗去农药残留,同时L-半胱氨酸具有很好的解毒中和生物中和能力,能够与无法洗去的农药残留中和,与十二烷基硫酸钠配合使用能够彻底去除农药残留影响;L-抗坏血酸具有强大的抗氧化作用,能够防止迷迭香的氧化变质有效成分丧失。
3)本发明使用改性的海藻糖,使得海藻糖的比表面积增大,包裹能力增强,在冻干时能防止迷迭香的有效组分随水蒸汽一起升华逸散,并使有效组分成形,对于迷迭香的冻干保护力最强,并且,在提取中,本发明使用低毒对环境无害的丙三醇作为提取液主要成分,配合L-抗坏血酸对迷迭香冻干粉进行浸出,绿色环保,同时能够最大程度保留有效活性成分。
综上的,本发明所述的方法相比现有技术,有机溶剂的使用量大大减少,最终产品中几乎没有乙醇残留,同时冻干流程短,节能减排,降低成本效果显著。
附图说明
图1为本发明冷冻干燥方法的流程示意图;
图2为实施例和对比例精油质量的比较;
图3为实施例和对比例中1g精油中β-蒎烯含量(mg);
图4为实施例和对比例中1g精油中中乙酸芳樟酯含量(mg)。
具体实施方式
如图1所示一种迷迭香的冷冻干燥方法,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-45~-55℃,压强300-800Pa,冻干30-60min;
B:-60~-55℃,压强150-250Pa,冻干100-200min;
C:-75~-85℃,压强70-150Pa,冻干30-45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:5-10的比例投入提取液中4-10℃浸泡12-24h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 10-20份
L-抗坏血酸 0.5-1份;
随后将含有迷迭香冻干粉提取液进行蒸馏提取获得迷迭香精油;
所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。
所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
所述步骤2)中的浸泡时间为2-6h,温度为15-30℃;
所述步骤7)中的冻干保护剂选自甘油,阿拉伯胶或海藻糖中的一种;
所述海藻糖经过如下步骤的改性:
a.称取海藻糖原料投入含有质量分数为1-3%氢氧化钠溶液中超声波清洗10-20min,随后放入质量分数0.5-1%的冰醋酸溶液中,对海藻糖溶液进行抽滤,然后用95%以上乙醇沉淀洗涤,干燥获得预处理海藻糖;
b.将预处理海藻糖与质量分数5-10%醋酸溶液加入反应容器,所述海藻糖原料与所述醋酸溶液的质量体积比为1g:5-10mL;冰水浴控制反应温度在0~5℃;在搅拌的状态下加入羟化卵磷脂;滴加完毕后撤去冰水浴,在室温下持续搅拌反应2~4h;经静置、沉淀、抽滤、干燥、重结晶得到改性海藻糖;其中所述预处理壳聚糖与羟化卵磷脂的质量比为1:(0.3~0.5)。
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
本发明实施例中使用的试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规试剂产品。
实施例1
一种迷迭香的冷冻干燥方法,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶,质量为1000g;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-45℃,压强300Pa,冻干30min;
B:-55℃,压强150Pa,冻干100min;
C:-75℃,压强70Pa,冻干30min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:5的比例投入提取液中4℃浸泡12h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 10份
L-抗坏血酸 0.5份;
随后将含有迷迭香冻干粉提取液进行蒸馏提取获得迷迭香精油;
所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。
所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
所述步骤2)中的浸泡时间为2-6h,温度为15-30℃;
所述步骤7)中的冻干保护剂选自甘油。
实施例2
一种迷迭香的冷冻干燥方法,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶,质量为1000g;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:50℃,压强500Pa,冻干45min;
B:-58℃,压强200Pa,冻干150min;
C:-80℃,压强133Pa,冻干40min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装。
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:8的比例投入提取液中8℃浸泡18h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 15份
L-抗坏血酸 0.75份;
随后将含有迷迭香冻干粉提取液进行蒸馏提取获得迷迭香精油;
所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。
所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
去离子水 100份
乙醇8份
葡萄糖酸氯己定3份
十二烷基硫酸钠2份
L-半胱氨酸 1.5份
L-抗坏血酸 0.75份;
所述步骤2)中的浸泡时间为2-6h,温度为15-30℃;
所述步骤7)中的冻干保护剂选自海藻糖;
所述海藻糖经过如下步骤的改性:
a.称取海藻糖原料投入含有质量分数为2%氢氧化钠溶液中超声波清洗15min,随后放入质量分数0.75%的冰醋酸溶液中,对海藻糖溶液进行抽滤,然后用95%以上乙醇沉淀洗涤,干燥获得预处理海藻糖;
b.将预处理海藻糖与质量分数7.5%醋酸溶液加入反应容器,所述海藻糖原料与所述醋酸溶液的质量体积比为1g:7.5mL;冰水浴控制反应温度在0~5℃;在搅拌的状态下加入羟化卵磷脂;滴加完毕后撤去冰水浴,在室温下持续搅拌反应2~4h;经静置、沉淀、抽滤、干燥、重结晶得到改性海藻糖;其中所述预处理壳聚糖与羟化卵磷脂的质量比为1:0.4。
实施例3
一种迷迭香的冷冻干燥方法,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶,质量为1000g;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-20~-40℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-55℃,压强800Pa,冻干60min;
B:-60℃,压强250Pa,冻干200min;
C:-85℃,压强150Pa,冻干45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:10的比例投入提取液中10℃浸泡24h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 20份
L-抗坏血酸 1份;
随后将含有迷迭香冻干粉提取液进行蒸馏提取获得迷迭香精油;
所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶;
所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
所述步骤2)中的浸泡时间为2-6h,温度为15-30℃;
所述步骤7)中的冻干保护剂选自阿拉伯胶。
对比例1
一种迷迭香的冷冻干燥方法,未使用保鲜清洗液对迷迭香清洗,而是使用去离子水,其他同实施例2。
对比例2
一种迷迭香的冷冻干燥方法,使用普通海藻糖,而不是使用实施例2中的改性海藻糖,其他同实施例2。
对比例3
一种迷迭香的冷冻干燥方法,未使用保鲜清洗液对迷迭香清洗,而是使用去离子水,使用普通海藻糖,而不是使用实施例2中的改性海藻糖,其他同实施例2。
测试例1
对实施例1-3以及对比例1-3的冷冻干燥方法提取获得迷迭香冻干粉,以及制备的精油进行比较,比较获得的冻干粉质量(g),获得的精油质量(g),用以代表冷冻干燥和精油提取的得率;1g精油中β-蒎烯含量(mg),1g精油中乙酸芳樟酯含量(mg),用以代表精油的质量,即冷冻干燥提取过程中对活性物质的保留能力,结果见表1和图2-4。
表1不同催化过程的反应结果
由表1的数据可知,对比例2和3的精油的质量较其余实施例减少较多,证明,经过本发明改性的海藻糖可以在冻干过程中较多的保留迷迭香中的精油成分。从表1中还可知,对比例1-3中精油中的β-蒎烯含量(mg)和乙酸芳樟酯含量(mg)相比实施例1-3由巨大的降低,证明本发明改性的海藻糖和保鲜清洗液综合作用,可以保留迷迭香中的活性成分。
上述实施例只是本发明的有限几种优选实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (7)
1.一种迷迭香的冷冻干燥方法,其特征在于,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%的迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-40~-20℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-55~-45℃,压强300-800Pa,冻干30-60min;
B:-60~-55℃,压强150-250Pa,冻干100-200min;
C:-85~-75℃,压强70-150Pa,冻干30-45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
所述步骤2)中的保鲜清洗液含有以下成分,按重量份数计包括:
所述步骤7)中的冻干保护剂选自海藻糖;
所述海藻糖经过如下步骤的改性:
a.称取海藻糖原料投入含有质量分数为1-3%的氢氧化钠溶液中超声波清洗10-20min,随后放入质量分数0.5-1%的冰醋酸溶液中,对海藻糖溶液进行抽滤,然后用95%以上乙醇沉淀洗涤,干燥获得预处理海藻糖;
b.将预处理海藻糖与质量分数5-10%的醋酸溶液加入反应容器,所述海藻糖原料与所述醋酸溶液的质量体积比为1g:5-10mL;冰水浴控制反应温度在0~5℃;在搅拌的状态下加入羟化卵磷脂;滴加完毕后撤去冰水浴,在室温下持续搅拌反应2~4h;经静置、沉淀、抽滤、干燥、重结晶得到改性海藻糖;其中所述预处理壳聚糖与羟化卵磷脂的质量比为1:(0.3~0.5)。
2.根据权利要求1所述的一种迷迭香的冷冻干燥方法,其特征在于,所述新鲜嫩叶为从迷迭香顶端向下茎杆20cm以内的新鲜嫩叶。
3.根据权利要求1所述的一种迷迭香的冷冻干燥方法,其特征在于,所述步骤2)中的浸泡时间为2-6h,温度为15-30℃。
4.根据权利要求1-3任一项所述的冷冻干燥方法制备获得的迷迭香。
5.一种迷迭香有效成分的提取工艺,其特征在于,包含如权利要求1-3任一项所述的冷冻干燥方法。
6.根据权利要求5所述的一种迷迭香有效成分的提取工艺,其特征在于,包括以下步骤:
1)迷迭香的采收:在3-11月上旬采收迷迭香的新鲜嫩叶;
2)迷迭香的保鲜清洗:使用保鲜清洗液对迷迭香新鲜嫩叶进行浸泡和清洗;
3)初步自然干燥:在通风阴凉处,温度为20-30℃条件下,对浸泡过的嫩叶进行自然干燥6-12h;
4)迷迭香粉碎:对干燥后的迷迭香进行机械粉碎,粉碎后的原料过100-200目筛,得到迷迭香粉;
5)烘干干燥:将迷迭香粉在30-50℃常压下进行进一步的烘干,使得含水量低于15%;
6)预冻:将上述含水量低于15%的迷迭香粉摊铺开,摊铺厚度在5-10cm,在常压下进行快速预冻,预冻时间30-60min,预冻温度-40~-20℃;
7)冷冻干燥:保持预冻温度的条件下,加入质量分数5-10%的冻干保护剂,与迷迭香粉充分混合后,放入冻干机进行冻干,冻干程序如下:
A:-55~-45℃,压强300-800Pa,冻干30-60min;
B:-60~-55℃,压强150-250Pa,冻干100-200min;
C:-85~-75℃,压强70-150Pa,冻干30-45min;
D:恢复到常温常压,获得迷迭香冻干粉,含水量低于5%,并真空包装;
8)迷迭香精油提取:将步骤7)获得的迷迭香冻干粉按质量比1:5-10的比例投入提取液中4-10℃浸泡12-24h,所述提取液由以下质量份数成分组成:
去离子水 100份
丙三醇 10-20份
L-抗坏血酸 0.5-1份;
随后将含有迷迭香冻干粉的提取液进行蒸馏提取获得迷迭香精油。
7.根据权利要求6所述的一种迷迭香有效成分的提取工艺制备获得的迷迭香精油。
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Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5084293A (en) * | 1990-06-26 | 1992-01-28 | Kalamazoo Holdings, Inc. | Activated ascorbic acid antioxidant compositions and carotenoids, fats, and foods stabilized therewith |
CN103966027A (zh) * | 2014-05-15 | 2014-08-06 | 嘉兴市得百科新材料科技有限公司 | 一种迷迭香复配提取物的制备方法 |
CN105601699A (zh) * | 2015-12-30 | 2016-05-25 | 胡丽 | 一种迷迭香中提取熊果酸的制备方法 |
KR20160116731A (ko) * | 2015-03-31 | 2016-10-10 | 유한회사 천향 | 로즈메리 추출물을 함유하는 비누 및 이의 제조방법 |
CN107032994A (zh) * | 2017-04-14 | 2017-08-11 | 广东丸美生物技术股份有限公司 | 一种迷迭香酸的提取工艺 |
CN107802547A (zh) * | 2017-12-06 | 2018-03-16 | 湖南省雅迭香科技有限公司 | 一种迷迭香洗发露 |
CN108739972A (zh) * | 2018-04-28 | 2018-11-06 | 杨凌农科大无公害农药研究服务中心 | 一种迷迭香壳聚糖保鲜组合物、制剂、制备方法及其应用 |
CN110786480A (zh) * | 2019-09-10 | 2020-02-14 | 丽江三川实业集团有限公司 | 一种风味冻干芒果的制备方法 |
CN113197303A (zh) * | 2021-06-07 | 2021-08-03 | 新疆驼闻天下生物科技有限公司 | 一种富含花色苷的沙棘冻干粉的制备方法 |
CN113796485A (zh) * | 2020-06-16 | 2021-12-17 | 沈阳恩柽研究院有限公司 | 一种农产品保鲜提取物及其应用 |
CN114246288A (zh) * | 2021-12-31 | 2022-03-29 | 浙江省园林植物与花卉研究所(浙江省萧山棉麻研究所) | 一种提高迷迭香物料中迷迭香酸保存效率的方法 |
WO2022142381A1 (zh) * | 2020-12-31 | 2022-07-07 | 东南大学 | 矿化微生物粉剂制备方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
PT110859B (pt) * | 2018-07-18 | 2021-06-29 | Inst Politecnico De Braganca | Obtenção de uma solução a partir de extratos de rosmarinus officinalis l. para utilização como revestimento alimentar. |
AU2021332201A1 (en) * | 2020-08-24 | 2023-05-04 | Food Nerd Inc. | Composition manufactured from freeze-dried embryonic sprouted plants, and methods of making and using the same |
-
2022
- 2022-10-21 CN CN202211292833.0A patent/CN115486530B/zh active Active
- 2022-10-27 WO PCT/CN2022/127867 patent/WO2024082329A1/zh unknown
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5084293A (en) * | 1990-06-26 | 1992-01-28 | Kalamazoo Holdings, Inc. | Activated ascorbic acid antioxidant compositions and carotenoids, fats, and foods stabilized therewith |
CN103966027A (zh) * | 2014-05-15 | 2014-08-06 | 嘉兴市得百科新材料科技有限公司 | 一种迷迭香复配提取物的制备方法 |
KR20160116731A (ko) * | 2015-03-31 | 2016-10-10 | 유한회사 천향 | 로즈메리 추출물을 함유하는 비누 및 이의 제조방법 |
CN105601699A (zh) * | 2015-12-30 | 2016-05-25 | 胡丽 | 一种迷迭香中提取熊果酸的制备方法 |
CN107032994A (zh) * | 2017-04-14 | 2017-08-11 | 广东丸美生物技术股份有限公司 | 一种迷迭香酸的提取工艺 |
CN107802547A (zh) * | 2017-12-06 | 2018-03-16 | 湖南省雅迭香科技有限公司 | 一种迷迭香洗发露 |
CN108739972A (zh) * | 2018-04-28 | 2018-11-06 | 杨凌农科大无公害农药研究服务中心 | 一种迷迭香壳聚糖保鲜组合物、制剂、制备方法及其应用 |
CN110786480A (zh) * | 2019-09-10 | 2020-02-14 | 丽江三川实业集团有限公司 | 一种风味冻干芒果的制备方法 |
CN113796485A (zh) * | 2020-06-16 | 2021-12-17 | 沈阳恩柽研究院有限公司 | 一种农产品保鲜提取物及其应用 |
WO2022142381A1 (zh) * | 2020-12-31 | 2022-07-07 | 东南大学 | 矿化微生物粉剂制备方法 |
CN113197303A (zh) * | 2021-06-07 | 2021-08-03 | 新疆驼闻天下生物科技有限公司 | 一种富含花色苷的沙棘冻干粉的制备方法 |
CN114246288A (zh) * | 2021-12-31 | 2022-03-29 | 浙江省园林植物与花卉研究所(浙江省萧山棉麻研究所) | 一种提高迷迭香物料中迷迭香酸保存效率的方法 |
Non-Patent Citations (3)
Title |
---|
Entrapment of rosemary extract by liposomes formulated by Mozafari method: physicochemical characterization and optimization.;Shima Jahanfar等;《Food Science & Technology》;第7卷(第12期);第1-3页 * |
迷迭香抗氧化成分乙醇浸提工艺优化及抗氧化性能研究;王莹等;《包装与食品机械》;第40卷(第4期);第8-13页 * |
迷迭香精油壳聚糖纳米粒的制备及在冷藏鱼肉中的应用研究;刘善智;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑(电子期刊)》(第01期);第B024-888页 * |
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