CN1100727A - 甜菊糖甙的精制方法 - Google Patents
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Abstract
一种用作食品添加剂的甜菊糖甙的精制方法，是
将粗制品水溶液用脂肪醇、或脂肪醇加稀释剂进行液
—液萃取，用水反萃取。将萃余相和反萃取得到的水
相分别进行浓缩干燥得精制的甜菊糖甙。本发明的
工艺流程简单，产品洁白，纯度都在90％以上，且无
异味。
Description
本发明涉及到一种食品添加剂的精制方法，特别是由甜叶菊的叶和茎中提取的甜菊糖甙的精制方法。
甜菊糖甙是从甜叶菊植物（Stevia Rebau diana）干叶和茎中提取的新型甜味剂，它是由八种皂甙组成的混合物，其中甜菊甙（Stevioside）约占60-80%，甜菊甙A（Rebaudioside A）约占10-30%，其余为甜菊甙B、C、D、E，Dulcoside和Steviobioside。
目前国内外市场上的甜菊糖甙产品多用树脂吸附法制得。这种方法，如日本专利特开昭64-25790和中国专利CN90 103875所揭示。树脂吸附法收率较高，能耗较低。但其缺点是：采用弱碱性阴离子交换树脂脱色，脱色效率低;如用普通强碱性阴离子交换树脂脱色，则该树脂在使用过程中极易中毒，从第二循环开始，脱色容量迅速降低，因此，用这种方法生产的产品常带微黄色。在高效液相色谱（HPLC）图上有较多的杂质峰，产品带有异味，总甙含量为74-85%。其次是用这种方法生产的产品纯度不能满足生产高级食品和饮料甜味剂要求，也不能满足用于生产d-葡萄糖基甜菊甙原料的要求。
中国专利CN90104544.6揭示了一种去除异味的方法，将甜菊甙产品用石油醚提取脱脂，再用无水乙醇溶解，氢氧化钙、氧化铝吸附。过滤，干燥，收率为80%。此法步骤多，试剂消耗多，工业生产有困难，收率偏低。日本专利特开昭62-65158中采用甲醇结晶法制得含甙量96.6%的产品。但本法需用大量有毒的甲醇，不利于安全生产，而品质优良的甜菊甙A则与杂质一起存在于母液中不易回收，使此法回收率低。日本专利特开昭56-109568中提出用总碳原子数为4至8（用C4-C8表示，以下同）的醚类，C4-C7的酯类或C1-C4的氯代烷类作溶剂来萃取固体甜菊甙浓缩物或其水溶液，但这些溶剂的萃取效率低，所得产品仍为淡黄色，产品纯度较低。
本发明的目的在于提供一种工艺简单，产品纯度高、无异味的甜菊糖甙的精制方法。
本发明是采用了溶剂萃取工艺进行纯化，也就是说用脂肪醇或脂肪醇加稀释剂的混合物进行液-液萃取，所说的脂肪醇是用总碳原子数为4至8（C4-C8表示，以下同）的正构或异构脂肪醇的单一化合物或二种以上上述醇的混合物作萃取剂。所说的稀释剂可以是C6-C10的烃类、C4-C8的羧酸酯类、C6-C8的酮类或C4-C8的醚类化合物中的单一物质或其任意混合物，有机相中醇类化合物的含量应为5-100%。萃取可以在5-60℃的温度下进行，两相接触相比（有机相/水相）为0.5-3，可以用错流萃取或逆流萃取，萃取级数通常为3-6级。将萃余水相减压浓缩、干燥可得总甙含量大于95%的甜菊糖甙。用去离子水对负载有机相进行反萃取，将反萃取水相减压浓缩、干燥可以得总甙含量大于90%的甜菊糖甙。使用后的有机相可用蒸馏法回收。
本发明与现有技术相比，工艺流程简单，所得产品无异味，在HPLC图上没有杂质峰，纯度大于90%以上。
为进一步说明本发明，下面是几个具体的实施例：
取干燥的甜叶菊干叶5公斤，加入50升自来水在70℃的热水中浸出1小时，共浸出三次，最后弃去残叶得122升浸出液，向浸出液内加入500克工业流酸亚铁，搅拌半小时，再加入10%的石灰乳至pH9，此时产生绿色沉淀，静置半小时，过滤除去沉淀得清液116升。将清液通过吸附树脂柱，粒内装有10升CO3型大孔吸附树脂（核工业北京化工冶金研究院产品），吸附完毕用25升70%乙醇洗脱吸附树脂柱，以洗脱吸附的甜菊甙，将此洗脱液通过脱盐柱和脱色柱以除去电解质和色素。脱盐柱内装有1升J101阳离子交换树脂（核工业北京化工冶金研究院产品），脱色柱内装有可1升RCO4阴离子交换树脂（核工业北京化工冶金研究院产品），再用2.5升70%乙醇冲洗脱盐、脱色柱，将流出液与经脱盐、脱色后的洗脱液合并。再将此溶液在蒸馏塔内蒸馏出乙醇和部分水份，得浓缩液4升，将此液分为4等份，分别进行下述操作。
对照例：取上述浓缩液1升，减压下浓缩干燥得138克带有微黄色粉末。按国家标准GB8270-87方法分析甙含量86%，消光度E1%370为0.120，HPLC，分析甙含量总和为86.5%，杂质峰占11%，产品有少量异味。
实施例1：取上述浓缩液1升作水相，用500毫升异戊醇和500毫升乙酸乙酯配制成的有机相，在萃取器内进行4段逆流萃取，萃余水相经减压浓缩，干燥得108克白色粉末，经HPLC分析总甙含量96.5%，其中甜菊甙占70%，甜菊甙A占22.5%，其余五种甙占4%，未见杂质峰。按GB8270-87分析甙含量95%，E1%370为0.040，产品无异味。
将有机相用水反萃取，反萃取水相经减压浓缩，干燥得白色粉末12克，按GB8270-87方法分析甙含量90%，E1%370为0.020，产品无异味。
实施例2：取上述浓缩液1升作水相，用500毫升丁醇与500毫升120号溶剂汽油配制成的有机相在萃取器内进行4段逆流萃取，萃余水相经减压浓缩，干燥得105克白色粉末，按GB8270-87方法分析甙含量95%，E1%370为0.045，产品无异味。将有机相用水反萃取，反萃取水相经减压浓缩，干燥得白色粉末14克，按GB8270-87方法分析甙含量90%，E1%3700.025，产品无异味。
实施例3：取上述浓缩液1升作水相，用250毫升仲丁醇，250毫升异戌醇和500毫升二丁基醚配制成的有机相，在萃取器内进行4段逆流萃取，萃余水相经减压浓缩，干燥得107克白色粉末，按GB8270-87方法分析甙含量97%，E1%370为0.041，产品无异味。将有机相用水反萃取，反萃取水相经减压浓缩，干燥得白色粉末12克，按GB8270-87方法分析甙含量91%，E1%370为0.020，产品无异味。
本发明总甙回收率大于90%。
Claims (2)
1、一种甜菊糖甙的精制方法，采用溶剂萃取工艺进行纯化，本发明的特征在于用脂肪醇、或脂肪醇加稀释剂对甜菊甙粗制品的溶液进行溶剂萃取，负载有机相，用水反萃取，萃余水相和反萃取水相经浓缩、干燥得到高纯产品，所说的脂肪醇是指总碳原子数为4至8(用C4-C8表示，下述相同)的正构脂肪醇或异构脂肪醇的单一化合物或两种以上上述醇的混合物。所说的稀释剂是C6-C10的烃类、C4-C8的羧酸酯类、C4-C8的酮类或C4-C8的醚类化合物中的单一物质或其任意混合物。
2、按照权力要求1所说的一种甜菊糖甙精制的方法，其特征在于脂肪醇与稀释剂的混合物中，脂肪醇为5-100%。
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Cited By (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101194707B (zh) * | 2008-01-07 | 2010-10-20 | 青岛润德生物科技有限公司 | 高纯度甜菊糖甙的精制方法 |
| CN101503435B (zh) * | 2009-03-26 | 2011-07-06 | 李善汪 | 采用二次离子交换提纯甜菊糖甙的方法 |
| US8257948B1 (en) | 2011-02-17 | 2012-09-04 | Purecircle Usa | Method of preparing alpha-glucosyl Stevia composition |
| US8318459B2 (en) | 2011-02-17 | 2012-11-27 | Purecircle Usa | Glucosyl stevia composition |
| US8334006B2 (en) | 2005-10-11 | 2012-12-18 | Purecircle Sdn Bhd | Process for manufacturing a sweetener and use thereof |
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1993
- 1993-09-21 CN CN 93117563 patent/CN1032651C/zh not_active Expired - Fee Related
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