CN1243835A - 莱苞迪甙a提取方法 - Google Patents

莱苞迪甙a提取方法 Download PDF

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Publication number
CN1243835A
CN1243835A CN 98114220 CN98114220A CN1243835A CN 1243835 A CN1243835 A CN 1243835A CN 98114220 CN98114220 CN 98114220 CN 98114220 A CN98114220 A CN 98114220A CN 1243835 A CN1243835 A CN 1243835A
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glucoside
extracting method
general glycoside
resins exchange
secondary crystal
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CN 98114220
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程志军
田宏启
王熙恭
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Hailin Stevia Rebaudinum Sugar Co Ltd Heilongjiang Wasteland Reclaiming Regi
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Hailin Stevia Rebaudinum Sugar Co Ltd Heilongjiang Wasteland Reclaiming Regi
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Priority to CN 98114220 priority Critical patent/CN1243835A/zh
Publication of CN1243835A publication Critical patent/CN1243835A/zh
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Abstract

本发明提供了一种A3甙提取方法。甜菊糖甙总甙中含有st甙等有苦涩味成分,而A3甙的嗜口性较好,目前A3甙提取率较低。本发明的工艺以甜菊糖甙总甙为原料,先加入甲醇进行一次结晶处理,分离出st甙,再去除甲醇之后进行二次结晶处理,分离出R-C甙,提取出A3甙产品,其产品中A3甙的含量可达85—91%。纯度高,工艺方法的运行成本低。

Description

莱苞迪甙A提取方法
本发明涉及的是一种分离方法,特别是一种结晶方法。
甜菊糖甙总甙是从绿色植物-甜叶菊干叶中提取出来的食品添加剂-甜味剂。甜菊糖甙总甙由8种成份组成,其中含量最高的是st甙,称为甜菊甙stevioside,其甜度倍数是蔗糖的270-300倍,分子量为804.9,熔点为196-198℃,总甙中它的含量占64-70%。总甙中合有A3甙(又称为甜菊糖精甙A、莱苞迪甙A)Rebaudioside A,简称R-A,REA RED-A,其甜度倍数是庶糖的400-450倍,分子量为967.0,熔点为242-244℃,总甙中它的含量占22-28%。总甙中含有R-C甙(又称莱包迪甙C)RebaudiosideC简称R-C REC REB-C,其甜度倍数是蔗糖的40-60倍,分子量为951.0,熔点为215-217℃,总甙中它的含量占4-7%。总甙中含有R-D甙(又称莱包迪甙D)RebaudiosideD,简间称R-D,其甜度倍数是蔗糖的150-250倍,分子量为1129.2,熔点为283-286℃,总甙中它的含量占1%左右。总甙中合有R-E甙(又称莱包迪甙E)RebaudiosideE,简称R-E,其甜度倍数是蔗糖的100-150倍,总甙中它的含量占3%左右。其它三种甙元可忽略不计。st甙具有一定的苦涩味,影响总甙的口味,而A3甙嗜口性特别好。因此如何从总甙中分离出st甙提取A3甙是近年来研究的课题,但至此A3甙的提取纯度只能达到60-70%。
本发明之目的在于提供一种能够提高A3甙纯度的A3甙提取方法。
本发明的目的是这样实现的:
A.以甜菊糖甙总甙为原料,
B.向总甙中加入总甙重量2-2.5倍的甲醇,在常温常压下进行一次结晶,过滤去除st甙固形物,
C.滤液用树脂交换、分离出甲醇后再在常温常压下二次结晶,过滤所得滤液为所需产品,固形物为R-C甙。
为了控制结晶的速度和晶体的粒度,一次结晶和二次结晶均在有搅拌状态下进行。为了提高结晶体的纯度,提高提取率,一次结晶时间控制在18-24小时,二次结晶舍己救人控制在25-30小时。为了降低成本,树脂交换分离出的甲醇回流与总甙混合。
本发明的方法可以将具有苦涩味的st甙等成份分离出去,提取高纯度的A3甙,采用本发明的方法提取的产品中,A3甙的含量可达85-91%。提取后的A3甙具有良好的嗜口性。本发明工艺流程比较简单,消耗低,运行成本较低。
附图是本发明工艺流程图。
下面举例对本发明做更详细的描述:以甜菊糖甙总甙为原料,在总甙中加入重量是总甙2倍的甲醇,充分搅拌,在常温常压下进行20小时的一次结晶处理,过滤,滤饼制成粉状st甙,滤液用树脂交换,分离出甲醇,并将甲醇回流至与总甙原料相混配工序,滤液用在常温常压下、有充分搅拌的条件下进行28小时的二次结晶处理,二次结晶之后过滤,滤液制成R-C甙,滤饼制成粉状A3甙产品。

Claims (9)

1、一种A3甙提取方法,其特征是:
A.以甜菊糖甙总甙为原料,
B.向总甙中加入总甙重量2-2.5倍的甲醇,在常温常压下进行一次结晶,过滤去除st甙固形物,
C.滤液用树脂交换、分离出甲醇后再在常温常压下二次结晶,过滤所得滤液为所需产品,固形物为R-C甙。
2、根据权利要求1所述的A3甙提取方法,其特征是:一次结晶和二次结晶均在搅拌状态下进行。
3、根据权利要求1或2所述的A3甙提取方法,其特征是:一次结晶时间控制在18-24小时。
4、根据权利要求1或2所述的A3甙提取方法,其特征是:二次结晶时间控制在25-30小时。
5、根据权利要求3所述的A3甙提取方法,其特征是:二熔点熔点二次结晶时间控制在25-30小时。
6、根据权利要求1或2所述的A3甙提取方法,其特征是:树脂交换分离出的甲醇回流与总甙混合。
7、根据权利要求3所述的A3甙提取方法,其特征是:树脂交换分离出的甲醇回流与总甙混合。
8、根据权利要求4所述的A3甙提取方法,其特征是:树脂交换分离出的甲醇回流与总甙混合。
9、根据权利要求5所述的A3甙提取方法,其特征是:树脂交换分离出的甲醇回流与总甙混合。
CN 98114220 1998-08-05 1998-08-05 莱苞迪甙a提取方法 Pending CN1243835A (zh)

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WO2008091547A2 (en) 2007-01-22 2008-07-31 Cargill, Incorporated Method of producing purified rebaudioside a compositions using solvent/antisolvent crystallization
CN102030788A (zh) * 2011-01-05 2011-04-27 沈阳天峰生物制药有限公司 一种莱鲍迪苷c的制备方法
CN101270138B (zh) * 2007-03-23 2011-05-04 宁波绿之健药业有限公司 一种高含量甜菊糖a3甙的提取方法
WO2011094423A1 (en) 2010-01-28 2011-08-04 Cargill, Incorporated Methods to treat mixtures of glycosides to obtain one or more of these glycosides in more pure form
CN102144767A (zh) * 2010-02-10 2011-08-10 山东圣旺药业股份有限公司 一种80%含量莱鲍迪苷a的提取方法
US8017168B2 (en) 2006-11-02 2011-09-13 The Coca-Cola Company High-potency sweetener composition with rubisco protein, rubiscolin, rubiscolin derivatives, ace inhibitory peptides, and combinations thereof, and compositions sweetened therewith
CN101591366B (zh) * 2009-07-07 2012-05-30 天津美伦医药集团有限公司 分离高纯度瑞鲍迪甙a的工艺
CN102766176A (zh) * 2012-06-06 2012-11-07 天津北洋百川生物技术有限公司 一种结晶法提高甜菊糖总甙含量的方法
CN101309602B (zh) * 2005-11-23 2012-12-12 可口可乐公司 带有矿物质之高效甜味剂组成物及经彼甜化之组成物
EP2416670A4 (en) * 2009-04-09 2014-05-21 Cargill Inc SWEET COMPOSITION WITH REBAUDIOSIDE A HIGH SOLUBILITY FORM AND MANUFACTURING PROCESS
US9101160B2 (en) 2005-11-23 2015-08-11 The Coca-Cola Company Condiments with high-potency sweetener
US9131718B2 (en) 2009-06-16 2015-09-15 Epc (Beijing) Natural Products Co., Ltd. Process for rebaudioside D
US9578895B2 (en) 2010-08-23 2017-02-28 Epc (Beijing) Natural Products Co., Ltd. Rebaudioside A and stevioside compositions
US9795156B2 (en) 2011-03-17 2017-10-24 E.P.C (Beijing) Plant Pharmaceutical Technology Co., Ltd Rebaudioside B and derivatives
US10264811B2 (en) 2014-05-19 2019-04-23 Epc Natural Products Co., Ltd. Stevia sweetener with improved solubility
US10357052B2 (en) 2014-06-16 2019-07-23 Sweet Green Fields USA LLC Rebaudioside A and stevioside with improved solubilities
US10485256B2 (en) 2014-06-20 2019-11-26 Sweet Green Fields International Co., Limited Stevia sweetener with improved solubility with a cyclodextrin

Cited By (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9101160B2 (en) 2005-11-23 2015-08-11 The Coca-Cola Company Condiments with high-potency sweetener
CN101309602B (zh) * 2005-11-23 2012-12-12 可口可乐公司 带有矿物质之高效甜味剂组成物及经彼甜化之组成物
CN101500435B (zh) * 2005-11-23 2013-04-24 可口可乐公司 含有益生菌/益生素的高效甜味剂组成物以及利用彼所甜化之组成物
US8017168B2 (en) 2006-11-02 2011-09-13 The Coca-Cola Company High-potency sweetener composition with rubisco protein, rubiscolin, rubiscolin derivatives, ace inhibitory peptides, and combinations thereof, and compositions sweetened therewith
US8937168B2 (en) 2007-01-22 2015-01-20 Cargill, Incorporated Method of producing purified rebaudioside A compositions using solvent/antisolvent crystallization
WO2008091547A2 (en) 2007-01-22 2008-07-31 Cargill, Incorporated Method of producing purified rebaudioside a compositions using solvent/antisolvent crystallization
CN101270138B (zh) * 2007-03-23 2011-05-04 宁波绿之健药业有限公司 一种高含量甜菊糖a3甙的提取方法
EP2416670A4 (en) * 2009-04-09 2014-05-21 Cargill Inc SWEET COMPOSITION WITH REBAUDIOSIDE A HIGH SOLUBILITY FORM AND MANUFACTURING PROCESS
US9635878B2 (en) 2009-06-16 2017-05-02 Epc (Beijing) Natural Products Co., Ltd. Process for rebaudioside D
US9131718B2 (en) 2009-06-16 2015-09-15 Epc (Beijing) Natural Products Co., Ltd. Process for rebaudioside D
CN101591366B (zh) * 2009-07-07 2012-05-30 天津美伦医药集团有限公司 分离高纯度瑞鲍迪甙a的工艺
WO2011094423A1 (en) 2010-01-28 2011-08-04 Cargill, Incorporated Methods to treat mixtures of glycosides to obtain one or more of these glycosides in more pure form
CN102144767B (zh) * 2010-02-10 2012-10-10 山东圣旺药业股份有限公司 一种80%含量莱鲍迪苷a的提取方法
CN102144767A (zh) * 2010-02-10 2011-08-10 山东圣旺药业股份有限公司 一种80%含量莱鲍迪苷a的提取方法
US10285425B2 (en) 2010-08-23 2019-05-14 Epc Natural Products Co. Ltd Rebaudioside A and stevioside compositions
US11202462B2 (en) 2010-08-23 2021-12-21 Sweet Green Fields International Co., Limited Rebaudioside A and stevioside compositions
US9578895B2 (en) 2010-08-23 2017-02-28 Epc (Beijing) Natural Products Co., Ltd. Rebaudioside A and stevioside compositions
CN102030788A (zh) * 2011-01-05 2011-04-27 沈阳天峰生物制药有限公司 一种莱鲍迪苷c的制备方法
CN102030788B (zh) * 2011-01-05 2014-07-02 沈阳天峰生物制药有限公司 一种莱鲍迪苷c的制备方法
US9795156B2 (en) 2011-03-17 2017-10-24 E.P.C (Beijing) Plant Pharmaceutical Technology Co., Ltd Rebaudioside B and derivatives
US11510428B2 (en) 2011-03-17 2022-11-29 Sweet Green Fields International Co., Limited Rebaudioside B and derivatives
CN102766176A (zh) * 2012-06-06 2012-11-07 天津北洋百川生物技术有限公司 一种结晶法提高甜菊糖总甙含量的方法
US10264811B2 (en) 2014-05-19 2019-04-23 Epc Natural Products Co., Ltd. Stevia sweetener with improved solubility
US10561165B2 (en) 2014-05-19 2020-02-18 Sweet Green Fields International Co., Limited Stevia sweetener with improved solubility
US11206857B2 (en) 2014-05-19 2021-12-28 Sweet Green Fields International Co., Limited Stevia sweetener with improved solubility
US10357052B2 (en) 2014-06-16 2019-07-23 Sweet Green Fields USA LLC Rebaudioside A and stevioside with improved solubilities
US10568351B2 (en) 2014-06-16 2020-02-25 Sweet Green Fields USA LLC Rebaudioside A and stevioside with improved solubilities
US11241031B2 (en) 2014-06-16 2022-02-08 Sweet Green Fields Usa, Llc Rebaudioside A and stevioside with improved solubilities
US10485256B2 (en) 2014-06-20 2019-11-26 Sweet Green Fields International Co., Limited Stevia sweetener with improved solubility with a cyclodextrin

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