CN103923152B - 一种罗汉果甙v的提取方法 - Google Patents
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Abstract
一种罗汉果甙V的提取方法，以罗汉果鲜果为原料，经清洗、破碎，再按下述步骤提取：1)糖化鲜罗汉果；2)水提取和浓缩；3)沉降离心处理；4)大孔树脂吸附、分离，采用多树脂柱组选择吸附，并分段收集解析液，根据含量不同，分批次合并处理；5)离子交换树脂精制；6)浓缩、回收乙醇；7)硅胶精制；8)浓缩和喷雾干燥，获得终产品罗汉果甙V提取物。本发明工艺精制，实现了让罗汉果糖各种甙元在床层中达到分段富集的效果，提取出的罗汉果甙V纯度高、色泽优、口感纯正。<pb pnum="1" />
Description
技术领域
本发明涉及从天然植物中提取有效成分的方法，特别是一种从罗汉果中提取甜甙V的方法。
背景技术
当今人类存在对甜味食品的普遍偏好，吃糖类食品成为人们摄入能量的主要方式之一，然而由于大量摄取蔗糖能引起糖尿病、肥胖症、心脏病等各种成人病而成为社会问题。选择使用合适的甜味剂则无论是在我们的日常生活中还是在食品、饮料、医药工业中都具有非常重要的作用。
罗汉果是葫芦科植物，此果以其甜度著名，罗汉果的甜度来自于其主要成分的罗汉果皂甙，既可入药也可以作为食品的甜味剂。罗汉果的主要甜味成分为罗汉果甙V，它是一种无碳水化合物、无热量的甜味剂，其甜度约为蔗糖的300倍，且口感优良，风味独特，质量稳定，可作为一种通用的天然甜味剂，代替人工甜味剂如阿斯巴甜，安赛蜜等，而且罗汉果甙V在高温加热、烹饪或烧烤时也都不会影响其风味，因此可被广泛地应用于食品和饮料中作为配料。
目前，提取罗汉果甙V的方法虽然很多，但是罗汉果甙还存在着质量不稳定的情况，直接影响着消费者的使用，如其口感差异，含量差异，及其色泽均影响着罗汉果甙的市场推广。另外，在将罗汉果甙V作为甜味剂配料方面也还存在着低甜度和低卡路里难以兼得的缺陷。
发明内容
针对现有技术存在的不足，本发明的目的在于提供一种纯度高、色泽优、口感纯正的罗汉果甙V的提取方法。
为实现上述目的，本发明的技术方案是：一种罗汉果甙V的提取方法，以罗汉果鲜果为原料，经清洗、破碎，再按下述步骤提取：
1)糖化鲜罗汉果：将破碎后的鲜罗汉果放入糖化溶液中，经搅拌器搅拌均匀，保温放置，所述糖化溶液是由多聚半乳糖醛酸酶溶解于经过RO反渗透得到的超纯水而成的溶液；其中，多聚半乳糖醛酸酶占鲜罗汉果的重量＝5～10wt‰，超纯水的体积＝2000L，保温温度＝25～35℃，放置时间＝5h；
2)水提取和浓缩：先将糖化好后的鲜罗汉果用超纯水进行提取；再用自来水回流提取、过滤，共四次，合并四次提取滤液；然后将合并后的提取滤液在真空减压下浓缩；
3)沉降离心处理：将浓缩后的提取滤液经高速离心分离处理和沉降，获得离心收集液，其中，离心机速度＝3000～5000r/min，沉降离心分离时间＝1h；
4)大孔树脂吸附、分离：采用DA201型的大孔吸附树脂，将其装入树脂柱中，该树脂柱四个串联为一树脂柱组，料液上柱进行吸附；吸附结束后，用乙醇解析，收集解析液，在该解析过程中，根据泄漏液的体积，分阶段解析并进行分析，依据每个阶段的解析液中罗汉果甙V的含量，分别确定出其对应解析液的下一步处理工序；
5)离子交换树脂精制：预先将选用的酸性阳离子交换树脂和碱性阴离子交换树脂分别装入树脂柱；从步骤4)中确定出需进行阳、阴离子处理的解析液分别过阳、阴离子交换树脂进行处理；收集走完阳、阴离子交换树脂得到的精制液；经水洗后，合并所有流出液，包含步骤3)中未进行此步骤处理的解析液；其中，酸性阳离子交换树脂采用001×16苯乙烯强酸性阳离子，碱性阴离子交换树脂采用201×4OH强碱性阴离子，处理时解析液的流量＝2～3BV/h；
6)浓缩、回收乙醇：将上述处理过的解析液在真空减压、<70℃温度下浓缩成浓缩液，并回收溶剂乙醇，其中，将浓缩液浓缩至投料鲜罗汉果重量的0.5～1倍；
7)硅胶精制：预先将选定的硅胶装入树脂柱中，同时将所述浓缩液经纯化水稀释后，通过硅胶柱，去掉液体中的杂质以及罗汉果甜甙同系物，收集全部流出液；
8)浓缩和喷雾干燥：先用有机膜进行动态脱醇、脱水浓缩，再经二次浓缩，通过减压蒸馏浓缩至额定浓度10～18波美度，最后通过喷雾干燥，获得终产品罗汉果甙V提取物，其中，所述有机膜的膜孔径在20～100Α°之间。
较佳的是，所述步骤4)中，将多组所述树脂柱组并联设置，每组的吸附按照第一柱至第四柱依次进行，直到第四柱出甜时为止；组与组之间的吸附根据产品需求，进行选择性吸附和层析分离。
较佳的是，所述步骤4)中，所述料液上柱流量范围为0.1～5BV/h，吸附结束后，水洗流量范围为0.1～5BV/h，直至出水无色，该时间持续5～20h。
较佳的是，所述步骤4)中，水洗后，采用45-85％乙醇解析，收集醇含量≥50％的解析液；所述分阶段解析是指：携载具有不同粒径颗粒的解析液，在通过树脂时，不同粒径颗粒以不同时间段，随泄漏液通过树脂，对该不同时间段的泄漏液分别进行解析，并对各阶段收集到的解析液进行HPLC分析。
较佳的是，所述步骤7)中，所述硅胶比表面为300～500m2/g，孔容为0.70～0.90ml/g，所述稀释后浓缩液通过反相硅胶柱分离、洗脱，至无甜味止。
较佳的是，所述步骤2)中，所述用自来水回流提取、过滤四次都在85～100℃以上温度下进行，第一次加入原料4倍体积的自来水，提取时间为2h，过滤；滤渣进入第二次提取，加入原料2倍体积的自来水，提取时间为1.5h，过滤；滤渣进入第三次提取，加入原料重量3倍体积的自来水，提取时间为1.0h，过滤；滤渣进入第四次提取，加入原料重量1倍体积的自来水，提取时间为0.5h，过滤；所述真空减压，于65℃以下浓缩至投料鲜罗汉果重量的5倍。
与现有技术相比，本发明具有如下优点及效果：(1)选择吸附：大孔树脂吸附采用四个树脂柱串联为一组，多树脂柱组并联设置，从而在使用过程中，实际操作不会受到周期性清洗、再生以及原辐物料等外因的影响，既提高了生产效率，延长了树脂的使用寿命，又稳定的确保了产品质量。(2)分段收集解析液：在收集解析液时，分段收集，分别检测甜甙含量，根据含量不同，分批次合并处理，而不是通常将解析液全部收集在一起处理。从而可以有效地保证高甙含量的产品与中。低甙含量的批次产品分离，既保证了产品质量，缩短了工艺周期，又可根据需求，有选择性地提供相应产品。(3)综合效果明显：由于本发明工艺精制，实现了让罗汉果糖各种甙元在床层中达到分段富集的效果，提取出的罗汉果甙V纯度高、色泽优、口感纯正。
以下将结合实施例对本发明作进一步详细说明，该实施例仅用于解释本发明，并不对本发明的保护范围构成限制。
具体实施方式
实施例：
浸泡分两批，一批浸泡2000克罗汉果，另一批浸泡1800克罗汉果。两批分别过大孔树脂吸附和解析，然后将解析液合并作为一批，并根据检测甙v含量分类组合，单独进行精制，获得三个小批次成品。
1.1称取2000克罗汉果，置于20000ml、温度为80℃水中，浸泡5小时，经过滤得到浸泡液20500ml。
大孔树脂吸附、解析：解析液采取分段切除的方法(解析液情况总结如下表1)
表1
1.2第二批试验过程控制如下：
a.称取1800克罗汉果，置于18000ml、温度为80℃水中，浸泡5个小时，经过滤得到浸泡液18500ml。
b.大孔树脂吸附、解析：解析液采取分段切除的方法(解析液情况总结如下表2)
表2
1.3以上两批合并后分类进行精制，试验过程控制如下：
a.以上两批解析液中罗汉果甙V含量在40％以上的共六批合并一批，解析液合计：580ml，出精制液：570ml。批号为：TR-50/55-20131121；
b.以上两批解析液中罗汉果甙V含量在30％—40％之间的的共四批合并一批，解析液合计：1091ml，出精制液：1070ml。批号为：TR-30/50/55-20131121；
c.以上两批解析液中罗汉果甙V含量在20％—30％的共六批合并一批，解析液合计：623ml，出精制液：601ml。批号为：TR-45/50/55-20131121。
1.4浓缩：
a.TR-50/55-20131121，浓缩至固含量30％，出浓缩液：50.3ml；
b.TR-30/50/55-20131121，浓缩至固含量30％，出浓缩液：102.5ml；
c.TR-45/50/55-20131121，浓缩至固含量10％，出浓缩液59.7ml。
1.5碳处理
a.TR-50/55-20131121，加0.35g活性炭，得到碳处理液：45ml；
b.TR-30/50/55-20131121，加0.72g活性炭，出浓缩液：98ml；
c.TR-45/50/55-20131121，加0.42g活性炭，出浓缩液54ml。
1.6烘干：
a.由TR-50/55-20131121出成品：9.8克，罗汉果甙V含量：64.03％；
b.由TR-30/50/55-20131121出成品：12.3克，罗汉果甙V含量：60.63％；
c.由TR-45/50/55-20131121出成品：3.1克，罗汉果甙V含量：47.51％。
综合以上三小批次总重量为：25.2克，将其三小批混粉作为一批，计算罗汉果甙V的含量为：61.02％，收率为0.66％。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.一种罗汉果甙V的提取方法，以罗汉果鲜果为原料，经清洗、破碎，再按下述步骤提取：
1)糖化鲜罗汉果：将破碎后的鲜罗汉果放入糖化溶液中，经搅拌器搅拌均匀，保温放置，所述糖化溶液是由多聚半乳糖醛酸酶溶解于经过RO反渗透得到的超纯水而成的溶液；其中，多聚半乳糖醛酸酶占鲜罗汉果的重量＝5～10wt‰，超纯水的体积＝2000L，保温温度＝25～35℃，放置时间＝5h；
2)水提取和浓缩：先将糖化好后的鲜罗汉果用超纯水进行提取；再用自来水回流提取、过滤，共四次，合并四次提取滤液；然后将合并后的提取滤液在真空减压下浓缩；
3)沉降离心处理：将浓缩后的提取滤液经高速离心分离处理和沉降，获得离心收集液，其中，离心机速度＝3000～5000r/min，沉降离心分离时间＝1h；
4)大孔树脂吸附、分离：采用DA201型的大孔吸附树脂，将其装入树脂柱中，该树脂柱四个串联为一树脂柱组，料液上柱进行吸附；吸附结束后，用45-85％乙醇解析，收集解析液，在该解析过程中，根据泄漏液的体积，分阶段解析并进行分析，依据每个阶段的解析液中罗汉果甙V的含量，分别确定出其对应解析液的下一步处理工序；
5)离子交换树脂精制：预先将选用的酸性阳离子交换树脂和碱性阴离子交换树脂分别装入树脂柱；从步骤4)中确定出需进行阳、阴离子处理的解析液分别过阳、阴离子交换树脂进行处理；收集走完阳、阴离子交换树脂得到的精制液；经水洗后，合并所有流出液，包含步骤3)中未进行此步骤处理的解析液；其中，酸性阳离子交换树脂采用001×16苯乙烯强酸性阳离子，碱性阴离子交换树脂采用201×4OH强碱性阴离子，处理时解析液的流量＝2～3BV/h；
6)浓缩、回收乙醇：将上述处理过的解析液在真空减压、<70℃温度下浓缩成浓缩液，并回收溶剂乙醇，其中，将浓缩液浓缩至投料鲜罗汉果重量的0.5～1倍；
7)硅胶精制：预先将选定的硅胶装入树脂柱中，同时将所述浓缩液经纯化水稀释后，通过反相硅胶柱，去掉液体中的杂质以及罗汉果甜甙同系物，收集全部流出液；
8)浓缩和喷雾干燥：先用有机膜进行动态脱醇、脱水浓缩，再经二次浓缩，通过减压蒸馏浓缩至额定浓度10～18波美度，最后通过喷雾干燥，获得终产品罗汉果甙V提取物。
2.根据权利要求1所述的提取方法，其特征在于，所述步骤4)中，将多组所述树脂柱组并联设置，每组的吸附按照第一柱至第四柱依次进行，直到第四柱出甜时为止；组与组之间的吸附根据产品需求，进行选择性吸附和层析分离。
3.根据权利要求1所述的提取方法，其特征在于，所述步骤4)中，所述料液上柱流量范围为0.1～5BV/h，吸附结束后，水洗流量范围为0.1～5BV/h，直至出水无色，该时间持续5～20h。
4.根据权利要求1所述的提取方法，其特征在于，所述步骤4)中，水洗后，经45-85％乙醇解析，收集醇含量≥50％的解析液；所述分阶段解析是指：携载具有不同粒径颗粒的解析液，在通过树脂时，不同粒径颗粒以不同时间段，随泄漏液通过树脂，对该不同时间段的泄漏液分别进行解析，并对各阶段收集到的解析液进行HPLC分析。
5.根据权利要求1所述的提取方法，其特征在于，所述步骤7)中，所述硅胶比表面为300～500m2/g，孔容为0.70～0.90ml/g，所述稀释后浓缩液通过反相硅胶柱分离、洗脱，至无甜味止。
6.根据权利要求1所述的提取方法，其特征在于，所述步骤8)中，所述有机膜的膜孔径在20～100Α°之间。
7.根据权利要求1至6中任一权利要求所述的提取方法，其特征在于，所述步骤2)中，所述用自来水回流提取、过滤四次都在85℃以上温度下进行，第一次加入原料4倍体积的自来水，提取时间为2h，过滤；滤渣进入第二次提取，加入原料2倍体积的自来水，提取时间为1.5h，过滤；滤渣进入第三次提取，加入原料重量3倍体积的自来水，提取时间为1.0h，过滤；滤渣进入第四次提取，加入原料重量1倍体积的自来水，提取时间为0.5h，过滤；所述真空减压，于65℃以下浓缩至投料鲜罗汉果重量的5倍。
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| CN105580932B (zh) * | 2014-10-22 | 2021-11-30 | 可口可乐公司 | 制备具有不同味道的茶叶提取物的方法 |
| CN104530168B (zh) * | 2014-12-12 | 2016-08-03 | 黄晓 | 一种罗汉果苷v的工业化制备方法 |
| US11357246B2 (en) | 2015-10-29 | 2022-06-14 | Firmenich Incorporated | High intensity sweeteners |
| CN105255946A (zh) * | 2015-11-06 | 2016-01-20 | 深圳市深宝技术中心有限公司 | 一种酶解-超声波协同提取罗汉果鲜果提取物的方法 |
| CN105911175A (zh) * | 2016-04-15 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | 一种从罗汉果中提取罗汉果皂苷v的方法 |
| CN106235331A (zh) * | 2016-07-30 | 2016-12-21 | 南京正宽医药科技有限公司 | 一种龙眼的提取方法 |
| CN108276465B (zh) | 2017-03-14 | 2020-01-07 | 桂林莱茵生物科技股份有限公司 | 一种以亚临界水解吸附技术分离纯化罗汉果甜苷ⅴ的方法 |
| CN111108213A (zh) | 2017-05-03 | 2020-05-05 | 弗门尼舍公司 | 制备高强度甜味剂的方法 |
| CN107602653B (zh) * | 2017-10-09 | 2020-06-16 | 晨光生物科技集团股份有限公司 | 一种从鲜罗汉果中提取罗汉果甜苷的方法 |
| CN109247561A (zh) | 2018-09-06 | 2019-01-22 | 湖南绿蔓生物科技股份有限公司 | 一种从罗汉果中制备罗汉果甜味组合物的方法及其应用 |
| CN109320576B (zh) * | 2018-10-25 | 2020-09-08 | 晨光生物科技集团股份有限公司 | 一种高含量罗汉果苷v的生产方法 |
| CN110105458B (zh) * | 2019-03-25 | 2021-06-25 | 湖南华诚生物资源股份有限公司 | 从罗汉果甜苷提取废液中提取多糖和d-甘露醇的方法 |
| CN112617146A (zh) * | 2020-12-08 | 2021-04-09 | 江西海富生物工程有限公司 | 一种罗汉果风味浓缩汁及其制备方法 |
| CN114539330B (zh) * | 2022-02-16 | 2023-07-14 | 广西扶南东亚糖业有限公司 | 一种罗汉果甜甙的提取方法及其应用 |
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