CN112043733B - 一种水溶性银杏叶提取物的生产方法 - Google Patents
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Abstract
一种水溶性银杏叶提取物的生产方法,包括以下步骤:(1)用乙醇水溶液渗漉提取;(2)提取液浓缩、冷却;(3)离心、精滤除杂;(4)混合溶剂进行酯沉;(5)水沉;(6)脱酸;(7)干燥,得水溶性高内酯银杏叶提取物。所得水溶性高内酯银杏叶提取物,其黄酮含量≥24.0%,内酯含量≥10.0%,常温水溶度>10%,银杏酚酸≤1ppm。生产的银杏叶提取物不仅水溶性好,且大大提高了产品中内酯的含量;生产成本低,操作简便,适用于大规模化生产。
Description
技术领域
本发明涉及一种水溶性银杏叶提取物的生产方法。
背景技术
银杏叶,是银杏科植物银杏的叶,又名白果叶。据《食疗本草》记载,银杏叶可用于心悸怔忡、肺虚咳喘等病症治疗。银杏叶提取物(GBE)是从银杏科属植物的银杏干燥叶中提取纯化而成的一种淡黄色粉状物质,其含有黄酮类化合物、萜内酯类、银杏糖类、其他活性物质等营养成分。银杏叶提取物主要有以下保健功能:促进机体循环、抗氧化、延缓衰老、提高记忆力、 防治高血压、调节血糖。银杏叶提取物是目前世界公认的治疗、预防心脑血管疾病最理想的药物成份。
银杏叶提取物经脱银杏酸后无毒副作用,可广泛用于医药、食品、化妆品等领域。
目前,国内生产的银杏叶提取物产品多为脂溶性,而脂溶性的银杏叶提取物在经济价值、应用面和人体吸收等方面均不如水溶性银杏叶提取物。
现有水溶性银杏叶提取物,多是以市售标准银杏叶提取物为原料,通过溶解、冷沉或酶解等方式获得,市售标准银杏叶提取物基本都是以柱层析方法富集黄酮、内酯以及脱酸获得。由于树脂对黄酮和内酯的吸附性,通常,用柱层析方法富集生产银杏叶提取物,内酯收率较低,而通过重复提取、处理,对资源浪费极大。
CN 02113533.9公开了一种水溶性银杏叶提取物的生产工艺,该工艺在粗品制备水溶性提取物时,采用常规大孔树脂吸附,由于树脂对黄酮和内酯的吸附性,内酯与黄酮苷水溶解性等的差异都很大,采取该工艺很难同时保证内酯的含量及成品的水溶性,有效成分损失比较大,生产成本高。
CN200510003243.1公开了一种水溶性银杏叶提取物的生产方法,该工艺在粗品制备水溶性提取物时,采用搅拌提取,静置,过滤,加明胶水溶液进行沉淀,再静置,过滤,真空浓缩至干,再加无水乙醇溶解,过滤,真空浓缩并干燥,粉碎,制备水溶性GBE。由于内酯对水及甲醇、乙醇的稀溶液不溶或难溶,加上明胶的沉淀作用,有效成分,尤其是内酯损失比较大。也由于粗提取物的叶来源、品质及加工工艺的不同,造成成分差异很大,无法得到含量规格及相对可控的成品。
CN200810060422.2公开了一种水溶性银杏叶提取物的生产工艺,以银杏叶子为原料,常规工艺得提取后,以乙醇使其充分溶解后回收乙醇至稠膏,再加适量乙醇,提取2~4次后过滤,滤液浓缩至稠膏;将稠膏以纯化水提取2~4次,提取液冷却过滤,浓缩,干燥,即得水溶性银杏叶提取物。该工艺中因需经多次加热提取和浓缩过程,黄酮容易氧化而损失,多次的过滤过程也容易导致总内酯成分的损失,鞣质含量较高。
CN201811247088.1公开的高水溶性银杏叶提取物的制备方法,CN201610149596.0公开的水溶性银杏叶提取物的制备工艺及水溶性银杏叶提取物,CN201810341413.4公开的高水溶性银杏叶提取物的制备方法,都是以标准银杏叶提取物为原料通过溶解或酶解方式获得水溶性银杏叶提取物,重复生产处理造成对黄酮内酯的损耗以及能耗的浪费,生产成本高。
发明内容
本发明要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种生产成本低,有效活性成分回收率高,能耗低,适合大规模工业化生产的水溶性银杏提取物的生产方法。
本发明解决其技术问题采用的技术方案是,一种水溶性银杏提取物的生产方法,包括如下步骤:
(1)提取:以银杏苗叶为原料,将所述银杏叶粉碎后,用乙醇水溶液渗漉提取,得提取液;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩除乙醇,得浓缩液,冷却;
(3)离心、精滤除杂:将步骤(2)所得浓缩液采用卧螺离心,精滤,除掉杂质,得到精滤液;
(4)酯沉:将步骤(3)所得精滤液用混合溶剂进行酯沉,得到轻液和重液;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,浓缩过程中补水除有机溶剂,然后进行水沉,将水沉液离心、过滤,得过滤液;
(6)脱酸:步骤(5)所得过滤液用活性炭脱酸,然后过滤、浓缩,得到浓缩液;
(7)干燥:步骤(6)所得浓缩液进行干燥,得水溶性高内酯银杏叶提取物。
进一步,步骤(1)中,所述银杏叶为银杏叶苗叶,黄酮含量≥1.1%,内酯含量≥0.4%。
进一步,步骤(1)中,乙醇水溶液的浓度为40~80%,优选60~70%。
进一步,步骤(1)中,所述乙醇水溶液的用量为银杏苗叶质量的8~12倍,优选9~11倍。
进一步,步骤(1)中,提取的温度为60~90℃;优选70~85℃,更优选80℃。
进一步,步骤(2)中,浓缩是,将提取液真空加热浓缩至无乙醇,浓缩过程中补水2~3次;所得浓缩液的密度为1.1~1.2。
进一步,步骤(2)中,浓缩的温度为30~70℃,优选35~55℃,真空度为-0.06~-0.09Mpa。
进一步,步骤(2)中,浓缩液用循环水冷却至0~25℃,优选10~16℃。
进一步,步骤(3)中,卧螺离心机转鼓转速为2500~5000r/min。
进一步,步骤(3)中,所述精滤采用两级精滤。
进一步,步骤(3)中,精滤用的精滤膜的孔径为2~10μm。目的是为了去除浓缩液中的油状沉淀以及不溶杂质。
进一步,步骤(4)中,混合溶剂为水饱和的乙酸乙酯或乙酸乙酯与乙醇混合,乙醇体积占比0~20%,优选5~10%;所述混合溶剂与浓缩液的体积比为6~9∶1。
进一步,步骤(4)中,酯沉的温度为25~65℃,优选35~55℃,更优选40~50℃;酯沉的时间≥20min,优选25-60min,更优选30-50min。酯沉的目的是富集银杏黄酮、内酯,除掉水中的蛋白质、鞣质等杂质。
进一步,步骤(5)中,水沉的温度为45~80℃,优选50~80℃,更优选60~70℃;水沉液含固率为5~15%,优选10~15%;水沉的时间为0.5~1.5h,优选0.8~1.2h;离心采用管分,管分转速:10000~20000r/min,过滤采用板框过滤,滤膜的孔径为0.45~0.8μm,目的是为了去除溶液中大部分的银杏酸以及水不溶性杂质。
进一步,步骤(6)中,所述活性炭的粒径为200~300目,用量为过滤液体积的0.1%~1.0%,脱酸的温度为50~90℃,优选70~90℃;脱酸的时间为0.5h~1.5h,优选0.8~1.2h。目的是,使用少量活性炭脱除溶液中残留的银杏酸;脱酸后过滤液真空加热浓缩至物料浓度为40%~50%。
进一步,步骤(7)中,所述干燥为喷雾干燥、低温冷冻干燥或水加热真空干燥;水加热真空干燥,温度控制在<80℃,真空度为-0.08~-0.09Mpa。
本发明方法采用混合溶剂酯沉,生产的银杏叶提取物不仅水溶性好,并且大大提高了产品中内酯的含量。采用物理方法进行脱酸,降低了生产成本,并且该工艺易于操作,生产周期短,能耗低,有效活性成分回收率高;适用于大规模化生产。所得产品中,总黄酮含量≥24.0%,内酯含量≥10.0%,常温水溶度>10%,银杏酚酸≤1ppm。
具体实施方式
以下结合实施例对本发明作进一步说明。
各实施例所得水溶性银杏提取物产品中,总黄酮醇苷、萜类内酯和总银杏酸的含量测定,按《中国药典》2015年版一部银杏叶提取物检查项下规定的检测方法进行。
实施例1
本实施例水溶性银杏提取物的生产方法,包括如下步骤:
(1)提取:称取所述银杏苗干叶(原料为陕西宁强2年苗叶6月采,黄酮含量1.35wt%,内酯含量0.56wt%)400Kg,粉碎后,用体积浓度75%的乙醇水溶液4800L进行渗漉提取,提取的温度为78~82℃;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩至无乙醇,浓缩过程中补水3次,浓缩的温度为48±2℃,真空度为-0.07~-0.08Mpa,得密度为1.1的浓缩液;
(3)离心、精滤除杂:将步骤(2)所得浓缩液冷却至小于20℃后,采用卧螺离心,卧螺离心机转鼓转速为3000r/min;将离心液进行两级精滤,精滤用的精滤膜的孔径为10μm,得精滤液;
(4)酯沉:将步骤(3)所得精滤液用水饱和的乙酸乙酯进行酯沉,得到轻液和重液;所述乙酸乙酯溶剂与浓缩液的体积比为9∶1,酯沉的温度为65℃;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,过程中补水3次,得100L物料,然后进行水沉,水沉的温度为70℃,水沉的时间为1.0h;将水沉液采用管分进行离心,管分转速15000r/min,流速控制在250L/h;将离心液采用板框过滤机进行过滤,滤膜的孔径为0.8μm,得过滤液;
(6)脱酸:步骤(5)所得过滤液用粒径为200目的活性炭脱酸,用量为过滤液体积的0.3%,脱酸的温度为90℃,时间为1.0h;然后板框过滤,真空加热浓缩,浓缩的温度为45~50℃,真空度为-0.07~-0.08Mpa,得到浓缩液,所述浓缩液的浓度为50.0%;
(7)干燥:步骤(6)所得浓缩液进行真空干燥,得水溶性高内酯银杏叶提取物9.5Kg,提取回收率2.38wt%,总黄酮含量25.57wt%,总内酯含量20.05wt%,银杏酸0.86ppm。
实施例2
本实施例水溶性银杏提取物的生产方法,包括如下步骤:
(1)提取:称取所述银杏苗干叶(原料为陕西宁强2年苗叶七月底采,黄酮含量1.18%,内酯含量0.52%)600Kg,粉碎后,用体积浓度70%的乙醇水溶液6000L进行渗漉提取,提取的温度76±1℃;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩至无乙醇,浓缩过程中补水2次,浓缩的温度为43±2℃,真空度为-0.08~-0.09Mpa,得密度为1.12的浓缩液;
(3)离心、精滤除杂:将步骤(2)所得浓缩液冷却至小于18℃后,采用卧螺离心,卧螺离心机转鼓转速为4000r/min;将离心液进行两级精滤,精滤用的精滤膜的孔径为10μm,得精滤液;
(4)酯沉:将步骤(3)所得精滤液用乙酸乙酯与乙醇的混合溶剂进行酯沉,乙醇体积占比5%,得到轻液和重液;所述乙酸乙酯溶剂与浓缩液的体积比为8∶1,酯沉的温度为60℃;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,过程中补水3次,得180L物料,然后进行水沉,水沉的温度为60℃,水沉的时间为1.0h;将水沉液采用管分进行离心,管分转速15000r/min,流速控制在300L/h;将离心液采用板框过滤机进行过滤,滤膜的孔径为0.8μm,得过滤液;
(6)脱酸:步骤(5)所得过滤液用粒径为300目的活性炭脱酸,用量为过滤液体积的0.25%,脱酸的温度为80℃,时间为1.0h;然后板框过滤,真空加热浓缩,浓缩的温度为45~50℃,真空度为-0.07~-0.08Mpa,得到浓缩液,所述浓缩液的浓度为48.3%;
(7)干燥:步骤(6)所得浓缩液进行喷雾干燥,得水溶性高内酯银杏叶提取物16.2Kg,提取回收率:2.7%,总黄酮含量:28.42%,总内酯含量:15.4%,银杏酸:0.75ppm。
实施例3
本实施例水溶性银杏提取物的生产方法,包括如下步骤:
(1)提取:称取所述银杏苗干叶(原料为陕西宁强2年苗叶8月采,黄酮含量1.19wt%,内酯含量0.47wt%)750Kg,粉碎后,用体积浓度65~68%的乙醇水溶液6750L进行渗漉提取,提取的温度72~75℃;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩至无乙醇,浓缩过程中补水2次,浓缩的温度为43±2℃,真空度为-0.08~-0.09Mpa,得密度为1.15的浓缩液;
(3)离心、精滤除杂:将步骤(2)所得浓缩液冷却至小于18℃后,采用卧螺离心,卧螺离心机转鼓转速为4000r/min;将离心液进行两级精滤,精滤用的精滤膜的孔径为10μm,得精滤液;
(4)酯沉:将步骤(3)所得精滤液用乙酸乙酯与乙醇的混合溶剂进行酯沉,乙醇体积占比10%,得到轻液和重液;所述乙酸乙酯溶剂与浓缩液的体积比为9∶1,酯沉的温度为45℃;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,过程中补水3次,得250L物料,然后进行水沉,水沉的温度为50℃,水沉的时间为1.0h;将水沉液采用管分进行离心,管分转速15000r/min,流速控制在300L/h;将离心液采用板框过滤机进行过滤,滤膜的孔径为0.8μm,得过滤液;
(6)脱酸:步骤(5)所得过滤液用粒径为200-300目的活性炭脱酸,用量为过滤液体积的0.5%,脱酸的温度为75℃,时间为1.0h;然后板框过滤,真空加热浓缩,浓缩的温度为45~50℃,真空度为-0.07~-0.08Mpa,得到浓缩液,所述浓缩液的浓度为45.2%;
(7)干燥:步骤(6)所得浓缩液进行真空干燥,得水溶性高内酯银杏叶提取物18.75Kg,提取回收率:2.5%,总黄酮含量:25.89%,总内酯含量:11.73%,银杏酸:0.32ppm。
Claims (2)
1.一种水溶性银杏叶提取物的生产方法,其特征在于,包括以下步骤:
(1)提取:称取银杏苗干叶400kg,粉碎后,用体积浓度75%的乙醇水溶液4800L进行渗漉提取,提取的温度为78-82℃;所述银杏苗干原料为陕西宁强2年苗叶6月采,黄酮含量1.35wt%,内酯含量0.56wt%;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩至无乙醇,浓缩过程中补水3次,浓缩的温度为48±2℃,真空度为-0.07~-0.08Mpa,得密度为1.1的浓缩液;
(3)离心、精滤除杂:将步骤(2)所得浓缩液冷却至小于20℃后,采用卧螺离心,卧螺离心机转鼓转速为3000r/min;将离心液进行两级精滤,精滤用的精滤膜的孔径为10μm,得精滤液;
(4)酯沉:将步骤(3)所得精滤液用水饱和的乙酸乙酯进行酯沉,得到轻液和重液;所述乙酸乙酯溶剂与浓缩液的体积比为9∶1,酯沉的温度为65℃;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,过程中补水3次,得100L物料,然后进行水沉,水沉的温度为70℃,水沉的时间为1.0h;将水沉液采用管式分离机进行离心,管式分离机转速15000r/min,流速控制在250L/h;将离心液采用板框过滤机进行过滤,滤膜的孔径为0.8μm,得过滤液;
(6)脱酸:步骤(5)所得过滤液用粒径为200目的活性炭脱酸,用量为过滤液体积的0.3%,脱酸的温度为90℃,时间为1.0h;然后板框过滤,真空加热浓缩,浓缩的温度为45-50℃,真空度为-0.07~-0.08Mpa,得到浓缩液,所述浓缩液的浓度为50.0%;
(7)干燥:步骤(6)所得浓缩液进行真空干燥,得水溶性高内酯银杏叶提取物9.5kg,提取回收率2.38wt%,总黄酮含量25.57wt%,总内酯含量20.05wt%,银杏酸0.86ppm。
2.一种水溶性银杏叶提取物的生产方法,其特征在于,包括以下步骤:(1)提取:称取所述银杏苗干叶600kg,粉碎后,用体积浓度70%的乙醇水溶液6000L进行渗漉提取,提取的温度76±1℃;所述银杏苗干叶原料为陕西宁强2年苗叶七月底采,黄酮含量1.18%,内酯含量0.52%;
(2)浓缩:将步骤(1)所得提取液进行真空加热浓缩至无乙醇,浓缩过程中补水2次,浓缩的温度为43±2℃,真空度为-0.08~-0.09Mpa,得密度为1.12的浓缩液;
(3)离心、精滤除杂:将步骤(2)所得浓缩液冷却至小于18℃后,采用卧螺离心,卧螺离心机转鼓转速为4000r/min;将离心液进行两级精滤,精滤用的精滤膜的孔径为10μm,得精滤液;
(4)酯沉:将步骤(3)所得精滤液用乙酸乙酯与乙醇的混合溶剂进行酯沉,乙醇体积占比5%,得到轻液和重液;所述乙酸乙酯溶剂与浓缩液的体积比为8∶1,酯沉的温度为60℃;
(5)水沉:将步骤(4)所得轻液真空加热回收溶剂,过程中补水3次,得180L物料,然后进行水沉,水沉的温度为60℃,水沉的时间为1.0h;将水沉液采用管式分离机进行离心,管式分离机转速15000r/min,流速控制在300L/h;将离心液采用板框过滤机进行过滤,滤膜的孔径为0.8μm,得过滤液;
(6)脱酸:步骤(5)所得过滤液用粒径为300目的活性炭脱酸,用量为过滤液体积的0.25%,脱酸的温度为80℃,时间为1.0h;然后板框过滤,真空加热浓缩,浓缩的温度为45~50℃,真空度为-0.07~-0.08Mpa,得到浓缩液,所述浓缩液的浓度为48.3%;
(7)干燥:步骤(6)所得浓缩液进行喷雾干燥,得水溶性高内酯银杏叶提取物16.2kg,提取回收率:2.7%,总黄酮含量:28.42%,总内酯含量:15.4%,银杏酸:0.75ppm。
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