CN110917294A - 一种高活性黄精膏的制备方法 - Google Patents
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Abstract
本发明提供了一种高活性黄精膏的制备方法,包括黄精活性成分提取、黄精酶水解转化反应、微孔膜过滤、减压浓缩、黄精活性成分二次转化等制备过程。黄精活性成分提取温度85~90℃,提取时间2~6h;黄精酶水解转化反应温度25~40℃,反应1~4h;微孔膜过滤压力为0.3~0.5MPa,膜过滤孔径1~5μm;减压浓缩温度60~75℃,真空度‑0.06~‑0.08Mpa,至固形物含量为30%~35%;黄精活性成分二次转化温度至85~90℃,常压搅拌保温8~12h,真空度‑0.05~‑0.07Mpa,进行减压浓缩,重复以上步骤,至固形物含量为60%~65%,浓缩结束,所得即为高活性黄精膏,较常规方法制备的黄精膏,本发明所述方法中黄精多糖及黄精甾体皂苷等活性成分含量提高30%以上。
Description
技术领域
本发明属于医药、保健食品、食品加工领域,特别提供一种高活性黄精膏的制备方法。
背景技术
黄精(Polygonatum sibiricum)为百合科多年生草本植物,根茎入药,至今已有两千多年的药用历史,最早见于晋代《名医别录》中记载。黄精性平、味甘,入脾、肾、肺经,具有补肾益精、宽中益气、滋阴润燥、生津补脾等功效,长期应用于脾胃虚弱、肾虚亏损、肺虚燥咳、体倦乏力等症的治疗。现代化学成分分析表明,黄精主要药效物质成分有甾体皂苷、多糖、低聚糖、三萜皂苷、黄酮等。黄精被列入***颁布的既是食品又是药品的物品名单中,安全性高。
目前国内外加工黄精的方式主要有以下几种方法:一是将黄精烘干后粉碎成颗粒,作为袋泡茶饮用;二是采用蒸晒结合的方法将黄精加工成制黄精,作为即食食品使用;三是利用有机溶剂及树脂吸附法单一分离黄精中多糖类或黄酮类成分,作为药品生产。以上加工工艺方法存在黄精有效成分和营养物质提取或转化程度低、技术方法落后、自动化程度低、产品食用方式不便捷等问题,难以保证产品应有的药用价值和保健功效,黄精规模化生产、标准化生产亟待解决,以促进黄精产业提档升级。
发明内容
为克服黄精现有加工技术中存在的加工工艺比较粗放、技术落后、自动化程度低、黄精高活性成分含量较低、食用不方便等问题,本发明研发了一种技术工艺路线成熟、黄精活性成分大幅提高、食用方便、自动化生产程度较高的一种高活性黄精膏的制备方法,以促进实现黄精规模化生产、标准化生产。
本发明技术方案如下:
一种高活性黄精膏的制备方法,其特征在于,具体步骤如下:
(1)黄精活性成分提取:清洗过的黄精进行切片,然后置于强制外循环式提取罐中,加入8~12倍黄精重量的纯化水,浸泡2~4h,开启蒸汽阀及循环泵,提取液温度达到85~90℃,动态循环提取,提取时间2~6h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)黄精酶水解转化反应:将暂存罐中的黄精提取液恒温至25~40℃,加入提取液重量1%~5%的新鲜黄精块,利用黄精块茎内存在的天然生物酶,保持25~40℃条件下1~4h,进行黄精酶水解转化反应;
(3)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.3~0.5MPa,把滤液输送到真空减压浓缩器;
(4)减压浓缩:控制真空减压浓缩器参数,浓缩温度60~75℃,真空度-0.06~-0.08Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为30%~35%Brix(w/w);
(5)黄精活性成分二次转化:将固形物含量为30%~35%Brix(w/w)的黄精浓缩液置于刮板式浓缩罐中,调整温度至85~90℃,常压搅拌保温8~12h,开启真空泵,调整真空度至-0.05~-0.07Mpa,进行减压浓缩;多次重复此步骤,至固形物含量为60%~65%Brix(w/w),浓缩结束,所得即为高活性黄精膏。
作为优选的技术方案:
步骤(1)中,黄精切片厚度为0.5~1cm。
步骤(2)中,新鲜黄精块的大小为边长0.5~1cm正方体或长方体。
步骤(3)中,所述微孔膜过滤器过滤孔径为1~5μm。
步骤(5)中,共进行三次常压搅拌保温+减压浓缩,第一次减压浓缩至固形物含量为40%~45%Brix(w/w),第二次减压浓缩至固形物含量为45%~50%Brix(w/w),第三次减压浓缩至固形物含量为60%~65%Brix(w/w)。
本发明所述黄精包括百合科植物滇黄精Polygonatum kingianum Coll.etHemsl、黄精Polygona-tum sibiricum Red.或多花黄精Polygonatum cyrtonema Hua的干燥根茎及其加工品。
本发明创造性的发明、使用了黄精活性酶水解反应技术、动态循环提取技术、黄精活性成分二次转化技术,所述加工技术更加先进,大大提高了黄精制品生产自动化控制程度,增加了产品的理化指标稳定性,使产品质量得到明显提高。本发明优化了高活性黄精膏的制备工艺参数,明确了黄精天然生物酶对黄精多糖、甾体皂苷与蛋白、淀粉等物质反应温度、时间,最大限度转化黄精多糖、甾体皂苷等高活性成分,有效提高了黄精膏中的高活性成分黄精多糖与黄精甾体皂苷的含量,其中黄精多糖含量≥6%,黄精甾体皂苷含量≥1.0%,较常规方法制备的黄精膏,其活性成分含量提高30%以上。本发明改变了黄精传统加工方法中蒸晒方法粗放、人工制作工序繁琐、质量品质标准化程度低等缺陷,本发明的实施有利于提高黄精产业的附加值,促进中药加工现代化的发展。
具体实施方式
实施例1
(1)黄精活性成分提取:清洗过的黄精切片,厚度0.5cm,置于强制外循环式提取罐中,加入8倍黄精重量的纯化水,浸泡2h,开启蒸汽阀及循环泵,提取液温度达到85℃,动态循环提取,提取时间2h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)黄精酶水解转化反应:将暂存罐中的黄精提取液恒温至25℃,加入提取液重量1%的新鲜黄精块,黄精块的大小为边长0.5cm的正方体,利用黄精块茎内存在的天然生物酶,保持25℃条件下1h,进行黄精酶水解转化反应;
(3)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.3MPa,膜过滤孔径1μm,把滤液输送到真空减压浓缩器中;
(4)减压浓缩:控制真空减压浓缩器参数,浓缩温度60℃,真空度-0.06Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为30%Brix(w/w);
(5)黄精活性成分二次转化:将固形物含量为30%Brix(w/w)的黄精浓缩液置于刮板式浓缩罐中,调整温度至85℃,常压搅拌保温8h,开启真空泵,调整真空度-0.05Mpa,进行减压浓缩,至固形物含量为40%Brix(w/w)。然后重复“调整温度至85℃,常压搅拌保温8h,开启真空泵,调整真空度-0.05Mpa,进行减压浓缩”步骤,至固形物含量为45%Brix(w/w)。再次重复“调整温度至85℃,常压搅拌保温8h,开启真空泵,调整真空度-0.05Mpa,进行减压浓缩”步骤,至固形物含量为60%Brix(w/w)。浓缩结束,所得即为高活性黄精膏,黄精多糖含量6.2%,黄精甾体皂苷含量1.1%。
实施例2
(1)黄精活性成分提取:清洗过的黄精切片,厚度1cm,置于强制外循环式提取罐中,加入12倍黄精重量的纯化水,浸泡4h,开启蒸汽阀及循环泵,提取液温度达到90℃,动态循环提取,提取时间6h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)黄精酶水解转化反应:将暂存罐中的黄精提取液恒温至40℃,加入提取液重量5%的新鲜黄精块,黄精块的大小为边长1cm的正方体,利用黄精块茎内存在的天然生物酶,保持40℃条件下4h,进行黄精酶水解转化反应;
(3)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.5MPa,膜过滤孔径5μm,把滤液输送到真空减压浓缩器中;
(4)减压浓缩:控制真空减压浓缩器参数,浓缩温度75℃,真空度-0.08Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为35%Brix(w/w);
(5)黄精活性成分二次转化:将固形物含量35%Brix(w/w)的黄精浓缩液置于刮板式浓缩罐中,调整温度至90℃,常压搅拌保温12h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩,至固形物含量为45%Brix(w/w)。然后重复“调整温度至90℃,常压搅拌保温12h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩”步骤,至固形物含量为50%Brix(w/w)。再次重复“调整温度至90℃,常压搅拌保温12h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩”步骤,至固形物含量为65%Brix(w/w)。浓缩结束,所得即为高活性黄精膏,黄精多糖含量6.1%,黄精甾体皂苷含量1.1%。
实施例3
(1)黄精活性成分提取:清洗过的黄精切片,厚度0.75cm,置于强制外循环式提取罐中,加入10倍黄精重量的纯化水,浸泡3h,开启蒸汽阀及循环泵,提取液温度达到90℃,动态循环提取,提取时间5h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)黄精酶水解转化反应:将暂存罐中的黄精提取液恒温至36℃,加入提取液重量3%的新鲜黄精块,黄精块的大小为边长0.75cm的正方体,利用黄精块茎内存在的天然生物酶,保持36℃条件下4h,进行黄精酶水解转化反应;
(3)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.5MPa,膜过滤孔径5μm,把滤液输送到真空减压浓缩器中;
(4)减压浓缩:控制真空减压浓缩器参数,浓缩温度70℃,真空度-0.06Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为32%Brix(w/w);
(5)黄精活性成分二次转化:将固形物含量为32%Brix(w/w)的黄精浓缩液置于刮板式浓缩罐中,调整温度至88℃,常压搅拌保温10h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩,至固形物含量为42%Brix(w/w)。然后重复“调整温度至88℃,常压搅拌保温10h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩”步骤,至固形物含量为50%Brix(w/w)。再次重复“调整温度至88℃,常压搅拌保温10h,开启真空泵,调整真空度-0.07Mpa,进行减压浓缩”步骤,至固形物含量为62%Brix(w/w)。浓缩结束,所得即为高活性黄精膏,黄精多糖含量7.0%,黄精甾体皂苷含量1.2%。
对比例
(1)黄精活性成分提取:清洗过的黄精切片,厚度0.75cm,置于强制外循环式提取罐中,加入10倍黄精重量的纯化水,浸泡3h,开启蒸汽阀及循环泵,提取液温度达到90℃,动态循环提取,提取时间5h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.5MPa,膜过滤孔径5μm,把滤液输送到真空减压浓缩器中;
(3)减压浓缩:控制真空减压浓缩器参数,浓缩温度70℃,真空度-0.06Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为65%Brix(w/w),所得即为黄精膏,黄精多糖含量3.5%,黄精甾体皂苷含量0.6%。
本发明未尽事宜为公知技术。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种高活性黄精膏的制备方法,其特征在于,具体步骤如下:
(1)黄精活性成分提取:清洗过的黄精进行切片,然后置于强制外循环式提取罐中,加入8~12倍黄精重量的纯化水,浸泡2~4h,开启蒸汽阀及循环泵,提取液温度达到85~90℃,动态循环提取,提取时间2~6h;过滤后的黄精残渣按上述工艺参数再提取一次,合并两次提取液,置于暂存罐中;
(2)黄精酶水解转化反应:将暂存罐中的黄精提取液恒温至25~40℃,加入提取液重量1%~5%的新鲜黄精块,利用黄精块茎内存在的天然生物酶,保持25~40℃条件下1~4h,进行黄精酶水解转化反应;
(3)微孔膜过滤:将上述提取液高压输送并通过微孔膜过滤器,输送泵压力为0.3~0.5MPa,把滤液输送到真空减压浓缩器;
(4)减压浓缩:控制真空减压浓缩器参数,浓缩温度60~75℃,真空度-0.06~-0.08Mpa,对黄精转化提取液进行减压浓缩,至固形物含量为30%~35%Brix(w/w);
(5)黄精活性成分二次转化:将固形物含量为30%~35%的黄精浓缩液置于刮板式浓缩罐中,调整温度至85~90℃,常压搅拌保温8~12h,开启真空泵,调整真空度至-0.05~-0.07Mpa,进行减压浓缩;多次重复此步骤,至固形物含量为60%~65%,浓缩结束,所得即为高活性黄精膏。
2.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:步骤(1)中,黄精切片厚度为0.5~1cm。
3.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:步骤(2)中,新鲜黄精块的大小为边长0.5~1cm正方体或长方体。
4.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:步骤(3)中,所述微孔膜过滤器过滤孔径为1~5μm。
5.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:步骤(5)中,共进行三次常压搅拌保温+减压浓缩,第一次减压浓缩至固形物含量为40%~45%,第二次减压浓缩至固形物含量为45%~50%,第三次减压浓缩至固形物含量为60%~65%。
6.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:所述黄精包括百合科植物滇黄精、黄精或多花黄精的干燥根茎及其加工品。
7.按照权利要求1所述高活性黄精膏的制备方法,其特征在于:所得高活性黄精膏中,黄精多糖含量≥6%,黄精甾体皂苷含量≥1.0%。
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