CN114075163A - 一种水热酸控浸提紫苏梗中木犀草素的方法 - Google Patents
一种水热酸控浸提紫苏梗中木犀草素的方法 Download PDFInfo
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- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
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- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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Abstract
本发明属于天然产物中活性成分提取技术领域,具体涉及一种水热条件下柠檬酸调控提取紫苏梗中木犀草素的方法。本发明以紫苏梗为原料,经水热酸控处理紫苏梗、紫苏梗活性成分的溶出、木犀草素制备的简单工艺而得到产品。本发明利用溶剂亚临界状态下产生高活性物质优势,提高植物纤维组织水解能效,降低天然活性物质传质阻力,并利用柠檬酸中H+调控溶出的天然活性物质的稳定性,提高木犀草素等活性成分提取能效。本发明方法原料来源广,木犀草素产品提取量高,操作步骤少,设备腐蚀小,有机溶剂使用量少,绿色环保等特点。本发明还可广泛应用于从紫苏梗中提取迷迭香酸、阿魏酸、香草醛及果胶等天然产物,有效实现了紫苏梗的资源化利用。
Description
技术领域
本发明属于木犀草素提取技术领域,具体涉及水热条件柠檬酸调控浸提紫苏梗中木犀草素方法。
背景技术
木犀草素( Luteolin) 是一种天然黄酮类化合物,多以糖苷形式存在于紫苏及其紫苏梗、花生、金银花等植物中,具有较强的抗氧化、抗炎、抗菌等功效,被广泛应用于食品、医药等行业。目前木犀草素提取方法有有机溶剂法、超声法、酶解法等,存在提取率不高、有机溶剂使用污染环境、目标物结构易破坏等问题。因此,研究一种高效、环保的提取木犀草素方法对提升紫苏梗资源利用价值具有重要现实意义。
现有2017年4月26日公开的发明专利CN 106588848 A“一种花生壳中提取木犀草素的方法”,公开的方法是:以花生壳粉末为原料,按花生壳粉末、溶剂和增溶剂质量1:6~18:0.01~0.1的比例,先用无水乙醇、丙酮或pH8~12的碱水溶液溶解,再加入聚乙烯吡咯烷酮、1-甲基-2-吡咯烷酮、1-乙基-2-吡咯烷酮和乳酸乙酯中的一种增溶剂,在20~60℃下搅拌4~8h,减压抽滤,滤饼重复提取2~4次,合并数次提取的滤液,用活性炭脱色30min,滤液旋转蒸发至浸膏状,浸膏碾碎,用水洗涤3~5遍干燥后得木犀草素粗品粉末,其木犀草素提取率为1.23%~1.36%,纯度为23.2%~38.2%。该方法的主要缺点是:(1)生产过程使用溶剂为无水乙醇、丙酮或pH8~12的碱水溶液,其中使用的碱易腐蚀设备,加大环境治理成本;有机溶剂丙酮易燃、易挥发性和慢性毒性对人体健康和环境造成威胁,加大生产的安全隐患,增加安全生产成本;(2)所选增溶剂为聚乙烯吡咯烷酮、1-甲基-2-吡咯烷酮、1-乙基-2-吡咯烷酮、乳酸乙酯等有毒、易燃的有机溶剂,影响木犀草素的品质,且增加木犀草素分离、纯化的工序,增加生产设备,从而增加生产成本;(3)产品生产过程中搅拌4~8h,有机溶剂重复提取3~4次,纯水3~5遍洗涤,生产步骤共7步,操作工序繁琐且耗时长,增加生产时间和设备占有,进一步增加生产成本。
发明内容
本发明的目的是,针对现有紫苏梗中木犀草素提取方法的不足,提供一种水热酸控浸提木犀草素的方法,具有有机溶剂使用量少、木犀草素溶浸充分且稳定、环境污染小、操作简单、生产成本低等特点。
本发明机理是:水热反应釜的高温(压)(温度介于 100 ℃~374 ℃之间)促使溶剂水处于亚临界状态,水的介电常数、表面张力和极性都显著降低,提高木犀草素溶解性和传质系数;升高温度致使提取体系内饱和蒸汽压升高,有助于提高水对植物纤维穿透能力,破坏组织致密结构,减少天然产物浸出的传质阻力。同时,水热反应体系产生的羟基自由基与纤维素中糖苷键发生氧化还原反应,减少细胞壁与细胞质间的传质屏障;柠檬酸中H+调控溶出的天然活性物质的稳定性,提高木犀草素等活性成分溶出能效。
实现发明目的的技术方案是:一种水热酸控浸提紫苏梗中木犀草素的方法,以紫苏梗粉末为原料,经水热酸控处理紫苏梗、紫苏梗活性成分的溶出、木犀草素产品制备的简单工艺而得到产品。所述方法的具体步骤如下:
(1)水热酸控处理紫苏梗
以紫苏梗(包括紫苏种植、紫苏叶加工过程产生的下脚料等)为原料,先称取清洗、烘干、粉碎后的紫苏梗粉末2~10g于水热反应釜中,再按照原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.1~1∶10~30的比例加入反应釜中,然后将反应釜放入150~250℃的烘箱中水热反应40~160min后取出冷却至室温,得紫苏梗反应液,所述乙醇溶液为体积分数为30%~70%的乙醇水溶液。
(2)紫苏梗活性成分的溶出
第(1)步完成后,先将紫苏梗反应液转入锥形瓶中,在超声波功率40~250 W、温度45~60 ℃条件下进行超声处理15~45 min后真空抽滤,分别收集滤液和滤渣,再将收集的滤液转入离心机中,在离心转速为2000~4000r/min条件下离心分离10~20min后,分别收集离心清液和离心渣,收集的离心液即为含木犀草素的提取液;收集的滤渣和离心渣作为制备吸附材料的原料。
(3)木犀草素产品制备
第(2)步完成后,先将收集的离心液定容后,采用高效液相色谱法测定离心液中木犀草素含量,色谱条件为流动相甲醇(ml)﹕磷酸溶液(ml)=35﹕65~60﹕40,温度25~35℃,进样量5~10μL,流速为0 .6~1ml/min,再将收集的离心液转入旋转蒸发器中,在真空压强为0.4~0.6 Mpa、温度为50~70℃下,进行减压浓缩得木犀草素浓缩液,最后将木犀草素浓缩液于冰箱中冷冻后,转移至真空冷冻干燥机中,干燥24~48h后,制得木犀草素粗制品,木犀草素提取量可达337.40~942.41ug/g,含量高达0.06~0.13%,所述磷酸溶液为0.1~0.5%。
本发明采用上述技术方案后,主要有以下效果﹕
(1)本发明通过水热反应降解植物组织纤维,再利用超声波协助有效活性成分溶出,柠檬酸调控天然活性物质的稳定性,促使木犀草素充分溶出且稳定,木犀草素浸提量最佳可达948.51ug/g,比未添加柠檬酸高4.2倍。
(2)本发明采用的紫苏梗经水热催化降解条件在1~2h最佳,柠檬酸添加量为1%,温度仅为230℃,操作简单,生产时间少,且使用的有机溶剂为乙醇,减少大量有毒有机溶剂在提取木犀草素的生产过程中的安全隐患,减少环境治理成本的同时,减少安全生产成本。
(3)本发明方法的原料来源广,紫苏梗利用充分,生产成本低,绿色环保,还可广泛提取其他活性成分,阿魏酸浸提量达276.17ug/g,迷迭香酸浸提量达167.49ug/g,香草醛浸提量达2.01mg/g,木犀草苷浸提量达332.20ug/g,实现了紫苏资源化利用。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明:
实施例1:
一种水热酸控浸提紫苏梗中木犀草素的方法的具体步骤如下:
(1)水热酸控处理紫苏梗
以紫苏梗(包括紫苏种植、紫苏叶加工过程产生的下脚料等)为原料,先称取清洗、烘干、粉碎后的紫苏梗粉末2g于水热反应釜中,再按照原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.42∶20的比例加入反应釜中,然后将反应釜放入230℃的烘箱中水热反应120min后取出冷却至室温,得紫苏梗反应液,所述乙醇溶液为体积分数为60%的乙醇水溶液。
(2)紫苏梗活性成分的溶出
第(1)步完成后,先将紫苏梗反应液转入锥形瓶中,在超声波功率250 W、温度60 ℃条件下进行超声处理30 min后真空抽滤,分别收集滤液和滤渣,再将收集的滤液转入离心机中,在离心转速为4000r/min条件下离心分离15min后,分别收集离心清液和离心渣,收集的离心液即为含木犀草素的提取液;收集的滤渣和离心渣作为制备吸附材料的原料。
(3)木犀草素产品制备
第(2)步完成后,先将收集的离心液定容后,采用高效液相色谱法测定离心液中木犀草素含量,色谱条件为流动相甲醇(ml)﹕磷酸溶液(ml)=35﹕65~60﹕40,温度30℃,进样量10μL,流速为1ml/min,再将收集的离心液转入旋转蒸发器中,在真空压强为0.5 Mpa、温度为70℃下,进行减压浓缩得木犀草素浓缩液,最后将木犀草素浓缩液于冰箱中冷冻后,转移至真空冷冻干燥机中,干燥48h后,制得木犀草素粗制品,木犀草素提取量可达942.41ug/g,含量高达0.13%,所述磷酸溶液为0.2%。
实施例2:
一种水热酸控浸提紫苏梗中木犀草素的方法,同实施例1,其中:
第(1)步中,原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.31∶10,反应温度为250℃,反应时间为100min,所述乙醇溶液为体积分数为50%的乙醇水溶液。
第(2)步中,超声温度为45℃,超声时间为45min,超声功率200w,离心转速为2000r/min,离心时间为20min。
第(3)步中,液相检测温度为25℃,进样量5μL,流速0.8ml/min,旋蒸压强为0.6Mpa、温度为60℃,冷冻干燥36h,木犀草素提取量可达484.21ug/g,含量高达0.08%,所述磷酸溶液为0.5%。
实施例3:
一种水热酸控浸提紫苏梗中木犀草素的方法,同实施例1,其中:
第(1)步中,原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.21∶15,反应温度为210℃,反应时间为60min,所述乙醇溶液为体积分数为40%的乙醇水溶液。
第(2)步中,超声温度为50℃,超声时间为15min,超声功率150w,离心转速为3000r/min,离心时间为10min。
第(3)步中,液相检测温度为35℃,进样量10μL,流速0.8ml/min,旋蒸压强为0.4Mpa、温度为50℃,冷冻干燥24h,木犀草素提取量可达337.40ug/g,含量高达0.08%,所述磷酸溶液为0.3%。
实验结果
1 .不同条件提取并制备木犀草素的实验结果如下 :
表1-1不同温度对木犀草素提取的影响
表1-2不同柠檬酸浓度对木犀草素溶出的影响
表1-3不同时间对木犀草素溶出的影响
从上述实验知:本发明采用水热酸控浸提紫苏梗中木犀草素,当紫苏梗在水热条件为230℃烘箱中烘120min时,其中加入1%的柠檬酸和40 ml的50%乙醇,木犀草素提取效果最佳,可达948.51ug/g,比未添加柠檬酸高4~6倍,且还检测出阿魏酸、迷迭香酸、香草醛、木犀草苷等活性成分,表明水热反应体系下柠檬酸调控有助于提高催化降解紫苏梗植物纤维能效,减少活性成分溶出的传质阻力,有利于天然活性成分的高效提取;水热提取过程中无其它有毒有害有机溶剂和浓酸强碱的使用,绿色环保,操作步骤简单,生产成本低。以上所述,仅为本发明所作的实施例,并非对本发明做任何形式上的限制,凡是依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化,均落入本发明的保护范围之列。
Claims (4)
1.一种水热酸控浸提紫苏梗中木犀草素的方法,其特征在于所述方法的具体步骤如下:
(1)水热酸控处理紫苏梗
以紫苏梗(包括紫苏种植、紫苏叶加工过程产生的下脚料等)为原料,先称取清洗、烘干、粉碎后的紫苏梗粉末2~10g于水热反应釜中,再按照原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.1~1∶10~30的比例加入反应釜中,然后将反应釜放入150~250℃的烘箱中水热反应40~160min后取出冷却至室温,得紫苏梗反应液,所述乙醇溶液为体积分数为30%~70%的乙醇水溶液;
(2)紫苏梗活性成分的溶出
第(1)步完成后,先将紫苏梗反应液转入锥形瓶中,在超声波功率40~250 W、温度45~60 ℃条件下进行超声处理15~45 min后真空抽滤,分别收集滤液和滤渣,再将收集的滤液转入离心机中,在离心转速为2000~4000r/min条件下离心分离10~20min后,分别收集离心清液和离心渣,收集的离心液即为含木犀草素的提取液;收集的滤渣和离心渣作为制备吸附材料的原料;
(3)木犀草素产品制备
第(2)步完成后,先将收集的离心液定容后,采用高效液相色谱法测定离心液中木犀草素含量,色谱条件为流动相甲醇(ml)﹕磷酸溶液(ml)=35﹕65~60﹕40,温度25~35℃,进样量5~10μL,流速为0 .6~1ml/min,再将收集的离心液转入旋转蒸发器中,在真空压强为0.4~0.6 Mpa、温度为50~70℃下,进行减压浓缩得木犀草素浓缩液,最后将木犀草素浓缩液于冰箱中冷冻后,转移至真空冷冻干燥机中,干燥24~48h后,制得木犀草素粗制品,木犀草素提取量可达337.40~942.41ug/g,含量高达0.06~0.13%,所述磷酸溶液为0.1~0.5%。
2.根据权利要求1所述水热酸控浸提紫苏梗中木犀草素的方法,其特征在于:
第(1)步中,原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.42∶20,水热温度为230℃,水热时间是120min,所述乙醇溶液为体积分数为60%的乙醇水溶液;
第(2)步中,超声温度为60℃,超声时间为30min,超声功率250w,离心转速为4000r/min,离心时间为15min;
第(3)步中,液相检测温度为30℃,进样量10μL,流速1ml/min,旋蒸压强为0.5 Mpa、温度为70℃,冷冻干燥48h,木犀草素提取量可达942.41ug/g,含量高达0.13%,所述磷酸溶液为0.2%。
3.根据权利要求1所述水热酸控浸提紫苏梗中木犀草素的方法,其特征在于:
第(1)步中,原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.31∶10,反应温度为250℃,反应时间为100min,所述乙醇溶液为体积分数为50%的乙醇水溶液;
第(2)步中,超声温度为45℃,超声时间为45min,超声功率200w,离心转速为2000r/min,离心时间为20min;
第(3)步中,液相检测温度为25℃,进样量5μL,流速0.8ml/min,旋蒸压强为0.6 Mpa、温度为60℃,冷冻干燥36h,木犀草素提取量可达484.21ug/g,含量高达0.08%,所述磷酸溶液为0.5%。
4.根据权利要求1所述水热酸控浸提紫苏梗中木犀草素的方法,其特征在于:
第(1)步中,原料质量(g)∶柠檬酸质量(g)∶乙醇溶液体积(ml)比为1∶0.21∶15,反应温度为210℃,反应时间为60min,所述乙醇溶液为体积分数为40%的乙醇水溶液;
第(2)步中,超声温度为50℃,超声时间为15min,超声功率150w,离心转速为3000r/min,离心时间为10min;
第(3)步中,液相检测温度为35℃,进样量10μL,流速0.8ml/min,旋蒸压强为0.4Mpa、温度为50℃,冷冻干燥24h,木犀草素提取量可达337.40ug/g,含量高达0.08%,所述磷酸溶液为0.3%。
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