CN112915040A - 一种低灰分、高水溶性的迷迭香提取物及其制备方法 - Google Patents
一种低灰分、高水溶性的迷迭香提取物及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种低灰分、高水溶性的迷迭香提取物及其制备方法。所述迷迭香提取物灰分≤3%;浓度为0.1%(m/v)时水溶液澄清透明,无悬浮和沉淀,浊度≤15FAU。所述迷迭香提取物制备方法包括酸性溶液提取、脱色、调pH、树脂纯化、浓缩、脱味、干燥等步骤。本发明提供的迷迭香提取物灰分低、水溶性好,有利于扩大其应用范围。
Description
所属技术领域
本发明涉及制药、食品、化妆品等日用品添加剂领域,具体涉及一种低灰分、高水溶性的迷迭香提取物及其制备方法。
背景技术
迷迭香是唇形科迷迭香属植物,又名“海洋之露”,“圣玛丽亚的玫瑰”,原产地中海地区,目前全世界许多地区都有种植,现在我国的贵州、湖南、广西等地均有规模化种植。迷迭香除是一种广泛使用的香料外,也具有很强的抗氧化活性,是目前全世界公认的具有较高抗氧化作用的一种植物。近年来,迷迭香抗氧化剂以其高效、广谱、耐热、安全等优良性能,在食品工业和一些相关行业的应用范围越来越宽。
迷迭香中主要抗氧化活性成分有二萜类、酚酸类和黄酮类物质。迷迭香酸(Rosmarinic acid,RA)是一种天然的具有多种生理活性的水溶性酚酸类化合物,具有极强的生物活性,如抗氧化、抗菌、消炎、抑制HIV整合酶、抑制透明质酸酶等活性。作为天然植物抗氧化剂,迷迭香酸具有极强的清除体内自由基活性,其抗氧化活性强于绿原酸、咖啡酸、叶酸等。迷迭香酸应用于化妆品行业可以抵抗紫外线,另外近几年迷迭香酸在医药、食品、保健品等领域已体现出其重要的应用价值。
由于迷迭香提取物主要应用于食品、化妆品及药品领域,水溶性差的迷迭香提取物会导致产品长时间放置后出现分层,底部有沉淀析出,影响产品的观感和使用效果。为了更好的实现迷迭香提取物的应用,寻找一种低灰分、水溶性好的迷迭香提取物及其制备方法显得尤为重要。
专利申请号CN201010130287.1公开了一种迷迭香酸的制备方法,采用水提与醇提结合、离子交换,置于层析分离介质上梯度洗脱,二次脱色、纳滤膜浓缩、重结晶制备迷迭香酸。
专利申请号CN201610886395.9公开了一种紫苏迷迭香酸的制备方法,将紫苏粉碎为粗粉状,利用70%的乙醇进行回流提取,提取液通过D101树脂吸附后,经醇洗得到一次洗脱液;将一次洗脱液通过NK109树脂吸附,经醇洗后得到二次洗脱液;将二次洗脱液进行活性炭脱色,调节脱色液pH值,利用乙酸乙酯反复萃取4次,取乙酸乙酯层液进行低温结晶及重结晶,晶体干燥后可得到含量为95-98%的迷迭香酸。
专利申请号CN201810008902.8公开了一种从迷迭香中提取迷迭香酸的工艺,包括以下步骤:S1、浸泡:迷迭香粉碎为粉状,然后利用乙醇浸泡;S2、提取:粉状的迷迭香用乙醇回流提取,经醇洗后得到一次洗脱液;S3、吸附:将一次洗脱液通过NK109树脂吸附,经醇洗后得到二次洗脱液;S4、结晶:然后将二次洗脱液进行活性岩石脱色,利用萃取剂反复萃取4-6次,取萃取剂层进行低温结晶及重结晶;S5、干燥:将上一步所得的晶体干燥后可得迷迭香酸。
上述提取方法工艺较为繁琐,产品收率较低,加工成本高,不利于工业化生产。并且,这些现有提取方法中均未涉及在提取和纯化过程中pH值的参数控制。本申请发明人发现,采用酸性乙醇提取,能够提高迷迭香酸提取物的收率,并且通过过程pH控制,得到的迷迭香酸提取物灰分低、水溶性好,有利于扩大其产品的应用范围。
发明内容
本发明的目的在于克服现有技术缺陷,提供一种具有低灰分、提高水溶性的迷迭香提取物及其制备方法,该方法制得的迷迭香提取物灰分≤3%,0.1%水溶液澄清透明,无悬浮或沉淀,浊度≤15FAU,在化妆品领域应用效果好,并且也有利于应用于食品、药品等领域。
具体而言,本发明产品主要是迷迭香原料经过提取、脱色、调pH、浓缩过滤、树脂吸附、解析液调pH、浓缩、干燥得到。
更进一步,本发明提取工艺包括以下步骤:(1)提取:取一定量迷迭香叶,经酸性乙醇提取、过滤后制得提取液;(2)脱色:向提取液中加入0.1%-1.5%的脱色剂,过滤后制得脱色液;(3)调pH:脱色液中添加pH调节剂调至pH4.0-6.5;(4)树脂纯化:调节pH后的脱色液浓缩、脱味过滤,滤液经大孔吸附树脂纯化获得解析液,解析液pH调节、浓缩、脱味、干燥,即得。
更进一步,上述步骤(1)的酸性乙醇中,所用酸为盐酸、磷酸、硫酸或其他无机酸,优选为磷酸,酸性乙醇提取剂的pH为2.8-4.0,优选为3.0-3.2。
更进一步,上述步骤(2)过程中所述的脱色剂为活性炭。
更进一步,上述步骤(3)和(4)中使用的pH调节剂为碱性溶液,优选为氨水;步骤(3)调节后溶液终pH进一步优选为4.0-5.5,更优选为4.0-4.5;步骤(4)调节后溶液终pH为4.0-5.5,优选为4.0-4.5。
更进一步,上述步骤(4)中将脱色液上柱并吸附完全后,先用纯水洗脱,然后再用60-80%乙醇溶液进行解析。解析用的乙醇溶液可进一步优选65%-75%;最优选为70%乙醇溶液。
本发明通过对制备工艺进行全面优化,尤其是对pH值的控制,以及调节pH所用的酸碱种类进行的优化,使得到的迷迭香提取物水溶性好、灰分低、易于应用。
本发明提供的迷迭香提取物灰分≤3%,水溶液澄清透明,无悬浮或沉淀,0.1%迷迭香酸水溶液浊度在15FAU以下。
本发明的有益效果是:(1)可获得低灰分、水溶性澄清透明的迷迭香酸产品;(2)制备方法简单,易于操作,时间短,效果显著;(3)通过调节pH既降低了产品灰分、提高了产品水溶性,并在一定程度上提高了产品的收率;(4)该方法得到的迷迭香酸水溶液澄清透明,在化妆品领域应用效果好。
附图说明
附图1显示本申请实施例1与市售样品2的溶解后的外观情况。图中左侧试管中溶解本发明迷迭香提取物;右侧试管中溶解市售迷迭香提取物。
附图2显示本申请实施例1与市售样品2的溶解并离心后的外观情况。图中左侧试管中溶解本发明迷迭香提取物;右侧试管中溶解市售迷迭香提取物。
图3显示经本发明制得的迷迭香酸和对比例2制得的迷迭香酸水溶效果图。左侧为对比例2制得的0.1%迷迭香酸的水溶效果;右侧为本发明制得的0.1%迷迭香酸的水溶效果。
具体实施方式
实施例1
取迷迭香叶(RA:1.48%)100g,经酸性乙醇(磷酸调至pH 2.8)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.0,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV70%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH至4.0,经浓缩、干燥后得到迷迭香提取物10.2g,纯度为11.96%,收率为82.4%。
实施例2
取迷迭香叶(RA:1.48%)100g,经酸性乙醇(磷酸调至pH 3.0)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.5,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV75%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH为4.0,经浓缩、干燥后得到灰分低、水溶性好的迷迭香提取物11.3g,纯度为10.50%,收率80.2%。
实施例3
取迷迭香叶(RA:1.48%)100g,经酸性乙醇(磷酸调至pH 3.2)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.0,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV65%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH为4.5,经浓缩、干燥后得到灰分低、水溶性好的迷迭香提取物10.5g,纯度为11.52%,收率81.7%。
实施例4
取迷迭香叶(RA:1.28%)100g,经酸性乙醇(磷酸调至pH 3.0)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.5,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV70%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH为4.0,经浓缩、干燥后得到灰分低、水溶性好的迷迭香提取物8.9g,纯度12.1%,收率84.1%。
实施例5
取迷迭香叶(RA:1.28%)100g,经酸性乙醇(磷酸调至pH 3.5)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.5,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV75%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH为5.5,经浓缩、干燥后得到灰分低、水溶性好的迷迭香提取物9.0g,纯度11.8%,收率83.0%。
实施例6
取迷迭香叶(RA:1.28%)100g,经酸性乙醇(磷酸调至pH 3.0)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用氨水调节pH为4.5,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV75%乙醇进行解析,解析流速为1BV/h,所获解析液用氨水调节pH为5.5,经浓缩、干燥后得到灰分低、水溶性好的迷迭香提取物9.2g,纯度11.3%,收率81.2%。
为了体现本申请制备方法的突出效果,制备以下对比例;与本申请实施例进行参数指标对比。
对比例1
取迷迭香叶(RA:1.48%)100g,经酸性乙醇(磷酸调至pH 2.8)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液用NaOH溶液调节pH为4.0,经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV70%乙醇进行解析,解析流速为1BV/h,所获解析液用NaOH溶液调节pH为4.0,经浓缩、干燥后得到迷迭香提取物11.1g,纯度10.98%,收率82.3%。
对比例2
取迷迭香叶(RA:1.48%)100g,经酸性乙醇(磷酸调至pH 3.0)提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV75%乙醇进行解析,解析流速为1BV/h,所获解析液经浓缩、干燥后得到迷迭香提取物8.9g,纯度10.21%,收率61.4%。
对比例3
取迷迭香叶(RA:1.48%)100g,经乙醇提取后得到迷迭香提取液,提取液中加入0.5%(m/v)的活性炭脱色后得到迷迭香脱色液,脱色液经浓缩、过滤得到迷迭香酸水溶液;迷迭香酸水溶液经LX-25M大孔吸附树脂上柱吸附,上柱液流速为1BV/h,待树脂吸附完全后,先用1.5BV纯水进行洗杂,然后用2BV75%乙醇进行解析,解析流速为1BV/h,所获解析液经浓缩、干燥后得到迷迭香提取物8.3g,纯度9.89%,收率55.5%。
1、提取物灰分及水溶性对比实验:
采用药典规定的灰分测定方法对实施例1-6、对比例1-3所得产品以及市售样品1、2进行测定,其中市售样品均为迷迭香酸含量10%的迷迭香提取物产品。
采用下述方法对实施例1-6、比例1-3所得产品以及市售样品1、2的水溶液的浊度进行测定。
称取0.1000g(精确至0.0001g)迷迭香提取物样品于100mL烧杯中,加50mL蒸馏水溶解,磁力搅拌器调29档,25℃搅拌5min,然后转移至100mL容量瓶中,用少量蒸馏水润洗烧杯,润洗液均转移至100mL容量瓶内,蒸馏水定容至刻度,摇匀后静置,待气泡消失后使用便携式比色计DR900进行检测,检测结果取整数。当检测结果≤12FAU时,在重复性条件下获得的两次独立测定结果的绝对差值≤2FAU。当检测结果≥12FAU时,重复性条件下获得的两次独立测定结果的绝对差值≤3FAU。
表1本发明部分实施例灰分、水溶性检测结果
以上结果表明,本申请方法制备获得的迷迭香提取物具有灰分低,澄清度好的技术效果。在不使用酸性乙醇;提取前后不控制pH值;或使用其他pH调节剂的情况下均无法达到本申请产品的优良参数指标。
2、应用效果对比:
1)实验方法
分别取实施例1制备的迷迭香提取物和市售样品2,按照0.1%的比例加入到市售护肤精华液中,在100-150rpm搅拌溶解5min,对比溶解效果;将溶液转移至离心管中并封盖,以4000rpm离心2min,对比溶液稳定性能。
2)实验结果
溶解性效果对比图如说明书附图图1所示,从图中可以看出采用本发明制得的迷迭香提取物在市售护肤精华液中应用溶解性较好,溶液无悬浮,澄清透亮。离心后的稳定性对比如见说明书附图图2,并从图中可以看出采用本发明制得的迷迭香提取物经离心后无沉淀析出,外观状态较好。
3、水溶效果比较
1)实验方法
分别取实施例1制备的迷迭香提取物和对比例2,按照0.1%的比例加入到水中,在100-150rpm搅拌溶解5min,对比溶解效果。
2)实验结果
水溶效果对比图如说明书附图图3所示,从图中可以看出采用本发明制得的迷迭香提取物水溶性较好,溶液无悬浮,澄清透亮。对比例2制备获得的迷迭香提取物在水中呈现出浑浊状态。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明保护的范围之内。
Claims (10)
1.一种低灰分、高水溶性的迷迭香提取物,其特征在于所述迷迭香提取物灰分≤3%,浓度为0.1%(m/v)时,水溶液澄清透明,无悬浮和沉淀,浊度≤15FAU。
2.根据权利要求1所述的一种低灰分、高水溶性的迷迭香提取物,其特征在于其制备方法包括以下步骤:
(1)提取:取一定量迷迭香叶,经酸性乙醇提取、过滤后制得提取液;
(2)脱色:向提取液中加入0.1%-1.5%的脱色剂,过滤后制得脱色液;
(3)调pH:向脱色液中添加pH调节剂调至pH4.0-6.5;
(4)树脂纯化:调节pH后的脱色液浓缩、脱味过滤,滤液经大孔吸附树脂纯化获得解析液,解析液pH调节、浓缩、脱味、干燥,即得。
3.根据权利要求2所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(1)所述的酸性乙醇中所用酸为盐酸、磷酸、硫酸或其他无机酸。
4.根据权利要求2-3任一项所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(1)所述的酸性乙醇提取剂的pH为2.8-4.0。
5.根据权利要求2-4任一项所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(3)、(4)中使用的pH调节剂为碱性溶液,优选氨水。
6.根据权利要求2-5任一项所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(3)中调节pH值至pH4.0-5.5。
7.根据权利要求2-6任一项所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(4)中将脱色液上柱并吸附完全后,先用纯水洗脱,然后再用60-80%乙醇溶液进行解析。
8.根据权利要求2-7任一项所述的低灰分、高水溶性的迷迭香提取物,其特征在于:步骤(4)解析液调节pH值至pH4.0-5.5。
9.权利要求1-8任一项所述的低灰分、高水溶性的迷迭香提取物作为化妆品原料的用途。
10.一种化妆品,其特征在于,含有权利要求1-8任一项所述的低灰分、高水溶性的迷迭香提取物。
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