WO2006038221A1 - Procede de production de steviosides a partir de stevia rebaudiana bertoni - Google Patents

Procede de production de steviosides a partir de stevia rebaudiana bertoni Download PDF

Info

Publication number
WO2006038221A1
WO2006038221A1 PCT/IN2004/000404 IN2004000404W WO2006038221A1 WO 2006038221 A1 WO2006038221 A1 WO 2006038221A1 IN 2004000404 W IN2004000404 W IN 2004000404W WO 2006038221 A1 WO2006038221 A1 WO 2006038221A1
Authority
WO
WIPO (PCT)
Prior art keywords
plant material
steviosides
treated
exchange resin
precipitate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/IN2004/000404
Other languages
English (en)
Inventor
Jonnala Kotesh Kumar
Garikapatidyva Kiran Babu
Vijay Kumar Kaul
Paramvir Singh Ahuja
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Council of Scientific and Industrial Research
Original Assignee
Council of Scientific and Industrial Research
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Council of Scientific and Industrial Research filed Critical Council of Scientific and Industrial Research
Publication of WO2006038221A1 publication Critical patent/WO2006038221A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20—Carbocyclic rings
    • C07H15/24—Condensed ring systems having three or more rings
    • C07H15/256—Polyterpene radicals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00—Processes for the preparation of sugar derivatives
    • C07H1/06—Separation; Purification

Definitions

  • the present invention relates to a process for the production of steviosides from Stevia rebaudiana Bertoni.
  • the present invention relates to a method for recovering steviosides from dried plant material of Stevia rebaudiana using ecofriendly extraction and purification procedures.
  • Water for extraction of the plant material and the ion exchange resins used in the present invention are ecofriendly, non-toxic in nature and are reusable which will ultimately have a tremendous impact on the process economics.
  • the yield of product obtained in the present invention is high and intensity of its sweetness is superior to the plant raw material with milky white in appearance. Background of the invention
  • the major drawbacks are that the precipitate was further used to produce steviosides by passing through strongly acidic ion exchange resin and subsequently with a weakly basic ion exchange resin at least for three to five times, which will not only increase the processing time but also affect the overall cost of production.
  • the overall yield of the end product could be low as the steviosides were recovered only from the precipitate instead from the filtrate and this fact was not mentioned any where in the patent specification.
  • the major drawbacks are that the solvent like methanol, which was used for extraction of the steviosides and precipitate steviosides, is harmful to humans and not recommended in the food products all over the world.
  • the steviosides extracts are passed through ion exchange resins without charging the feed and will not give good results and, therefore, this step is more time consuming with low yields.
  • the adsorbent resins used in this process are not advantageous until the stevioside solution is pretreated to remove the metal chelating and colouring impurities. Moreover, the stevioside solutions are needed to be eluted very slowly through these adsorbent resins.
  • a process for recovering diterpene glycosides from the Stevia rebaudiana plant includes the steps of sequentially extracting plant material with a first solvent of intermediate polarity to extract plant substances which tend to interfere with a liquid chromatographic separation of the glycosides, and then with a second solvent of high polarity to extract glycosides and chromatographically separating the extracted glycosides by introducing them onto a liquid chromatography column having a packing of an oxygen- containing organic stationary phase covalently bonded through a silicon atom to an inorganic support, eluting them with a solvent of polarity higher than that of the first solvent but lower than that of the second solvent, and collecting individually eluate fractions rich in respective glycosides.
  • the major drawbacks are use of a variety of solvents to extract and process steviosides, having different polarities including methanol which is toxic and not approved as food grade solvent.
  • Final purification of steviosides is achieved by loading crude steviosides on a column chromatography using adsorbents like silica gel as a stationary phase and eluting the column with the help of two solvents sequentially running through the column, which is not a commercially viable process.
  • a water- soluble organic solvent e.g., ethanol, acetone, etc. is dissolved in the solution having passed through the acidic cation exchange resin or an aqueous solution dissolving water-soluble organic solvent is passed through the basic anion exchange resin through which the aqueous solution containing stevioside has passed, and the stevioside is obtained from the passed solution.
  • the major drawbacks are the removal of water from aqueous extract, two stage successive treatment with basic and then with acid salts and solvent addition.
  • the treatment with ion exchanger resins and solvent removal at the end not only increases the number of processing steps but in turn increases the processing time and energy and also affects the overall economics of the production.
  • Sampath Kumar Method for recovery of stevioside; US Patent
  • the raw material preferably in comminuted form is first extracted with water, the resulting aqueous extract is treated with a di- or tricarboxylic acid chelating agent to remove metallic and other impurities as well as to lower the pH to less than about 4. Subsequently, a calcium-containing agent is added to precipitate out other impurities.
  • the aqueous extract is essentially neutralized with an acid and is then subjected to extraction with a water-immiscible solvent.
  • stevioside crystals are then recovered by cooling the water layer obtained from the said solvent extraction step.
  • the major drawbacks are that the aqueous extract is treated first with an acid and then with base and later neutralizing the solution and then treating with water immiscible solvents like n-butanol which will not only leave the salt residues in the aqueous solution but also suffer steviosides losses into n-butanol and also lower the yield of steviosides up on crystallization from concentrated aqueous solution.
  • the main object of the present invention is to provide a process for the production of steviosides from Stevia rebaudiana Bertoni, which obviates the drawbacks as detailed above.
  • Another object of the present invention is to provide a safer, ecofriendly and economically viable process for the production of steviosides.
  • Still another object of the present invention is to obtain purified steviosides in a fewer processing steps so as to reduce their time and cost of production.
  • Yet another object of the present invention is to generate efficient steam extraction methods to recover maximum steviosides from the plant material within shortest time.
  • the present invention provides a process for the production of steviosides from Stevia rebaudiana Bertoni, which comprises drying of plant material at temperature any where from 20 to 50 0 C, followed by pulverization to 20 to 400 mesh size, extracting the plant material in a solvent consisting of demineralised water and heating the contents by injecting the steam directly or indirectly to a temperature ranging from 50 0 C to 120 0 C.
  • the plant material was charged into the extraction tank along with, or without water.
  • the plant material was dipped in water for 0 (without dipping) to 1 day in the ratio of 1 : 1 to 1 :30.
  • extracting the dry or wet plant material by directly injecting steam for 0.25 to 4.0 hr. and the overall temperature of the contents were maintained between 50 0 C and 100 0 C.
  • the plant material is heated by directly injecting steam into the extracting tank in a continuous or non continuous mode.
  • the plant material is extracted for 1 to 3 times by directly injecting the steam till the ratio of plant raw material to cumulative water extracts falls from 1:10 to 1 :30.
  • the aqueous extract was treated with a basic salt containing divalent cation such as calcium hydroxide or calcium oxide or calcium chloride to form a precipitate.
  • a basic salt containing divalent cation such as calcium hydroxide or calcium oxide or calcium chloride.
  • the aqueous extract is basified at pH 8 to 10 to obtain a precipitate.
  • the base treated filtrate was optionally treated with neutral alumina to further remove colouring impurities.
  • the strongly acidic ion exchange resin employed was selected from gel type or macroporous type.
  • the weakly basic ion exchange resin employed was selected from gel type or macroporous type.
  • the anion exchange treated steviosides solution was optionally treated with neutral alumina to further remove colouring impurities.
  • the neutral alumina was washed with plenty of water before treating with steviosides solution.
  • the present invention provides a process for the production of steviosides from Stevia rebaudiana Bertoni.
  • the process comprises drying of plant material at temperature anywhere from 20 to 5O 0 C, followed by pulverization to 20 to 400 mesh size.
  • the plant material is then extracted in a solvent consisting of demineralised water and the contents heated by injecting steam directly or indirectly to a temperature ranging from 5O 0 C to 12O 0 C at a steam pressure ranging from 1 to 8 kg/cm 2 for 0.25 to 4.0 hr.
  • the plant material is then filtered to obtain an aqueous extract, which is then treated with basic salt to form a precipitate.
  • the treated extract is then filtered to separate a clear precipitate, which is then treated with ion exchange resins and thereafter, dried to obtain a product containing steviosides having stevioside in the range from 40 to 70%, Water is the only solvent employed throughout the process.
  • the plant material can be charged into the extraction tank along with or without water.
  • the plant material was dipped in water for 0 (without dipping) to 1 day in the ratio of 1:1 to 1:30.
  • the dry or wet plant material was extracted by directly injecting steam for 0.25 to 4.0 hr. and the overall temperature of the contents were maintained between 5O 0 C and 100 0 C.
  • the wet plant material is extracted by indirectly injecting steam for 0.25 to 4.0 hr. and the overall temperature of the contents were maintained between 5O 0 C and 100 0 C.
  • the plant material is tieated by directly injecting steam into the extracting tank in a continuous or non continuous 'mode.
  • the extraction is effected 1 to 3 times by directly injecting the steam till the ratio of plant raw material to cumulative water extracts falls from 1 :10 to 1:30.
  • the aqueous extract was treated with a basic salt containing divalent cation such as calcium hydroxide or calcium oxide or calcium chloride to form a precipitate.
  • the aqueous extract is basified at pH 8 to 10 to obtain a precipitate.
  • the base treated filtrate was optionally treated with neutral alumina to further remove colouring impurities.
  • the strongly acidic ion exchange resin employed was selected from gel type or macroporous type.
  • the weakly basic ion exchange resin employed was selected from gel type or macroporous type.
  • the anion exchange treated steviosides solution was optionally treated with neutral alumina to further remove colouring impurities.
  • Neutral alumina was washed with plenty of water before treating with steviosides solution.
  • Dry powder of Stevia rebctudiana plant material 20 to 400 mesh size cultivated in the institute farm was charged into hydro extraction unit along with water in the ratio of 1 :0 to 1:10 and heated the contents at 50° to 120° C for 0.25 to 4.0 hrs by directly or indirectly injecting steam, generated in a separate boiler at a pressure in the range of 1 to 8 kg/cm 2 .
  • the water extract was filtered to get rid off plant particles.
  • the aqueous extract containing colouring matter, steviosides and other compounds was treated with di- or tri- valent salts such as calcium hydroxide or calcium chloride or calcium oxide or aluminum salts or iron salts by maintaining the pH of the solution between 8 and 10 with continuous agitation for 2-5 minutes to obtain the precipitate.
  • the precipitate was separated by filtration and washed with plenty of fresh water. The washings were added to the filtrate and the filtrate was, optionally, treated with neutral alumina.
  • the separated filtrate was passed through a strong cation exchange resin and then through a weak anion, exchange resin. The flow rate in both these resins was maintained between 1 to 3 bed -volumes per hour.
  • the two resin columns were washed with fresh, tap water to recover the steviosides left in the column.
  • the final eluant obtained from anion resin was, optionally, treated with neutral alumina to remove further impurities.
  • the filtrate was dried to obtain purified steviosides.
  • the dried Stevia rebaudiana plant material was dipped/soaked in minimum amount of water just to wet the plant matrix; and heated the contents by directly injecting the steam with a high pressure 2-10 kg/cm 2 in order to extract the steviosides into the aqueous medium in an efficient way in a short time.
  • the steam directly injected into the extractor, surrenders its readily available latent heat onto the wet plant tissue so as to enable quick release of water soluble steviosides.
  • This method not only reduces the process time and enhances the extraction efficiency but also helps in reducing the cost of production.
  • the amount of water required to extract the plant material in a batch is very little compared to the conventional extraction methods. This in turn reduces the cost of,the extraction equipment.
  • the aqueous extract was treated with acid/base to precipitate and the precipitate/filtrate was further purified either with water niiscible/immiscible organic solvents or by treating with various synthetic polymeric adsorbent resins/ion exchange resins to obtain stevio sides.
  • trie aqueous extract is treated with an alkali only and the filtrate is directly subjected to gel/macroporous type strong cation exchanger resin and then to gel/macroporous type weak anion exchange resin.
  • Example-l One kilo gram of Stevia plant powder 200 to 400 mesh sizes was extracted with demineralised water (3 x 4L) at 70 to 80° C. The extract was cooled and filtered on a Wattman 40 filter paper. The filtrate having about 40% dissolved solids was treated with aqueous calcium hydroxide (50 gm in 50 ml distilled water) till the pH was attained to 9.2 at room temperature and stirred for half an hour to obtain a precipitate.
  • demineralised water 3 x 4L
  • the filtrate having about 40% dissolved solids was treated with aqueous calcium hydroxide (50 gm in 50 ml distilled water) till the pH was attained to 9.2 at room temperature and stirred for half an hour to obtain a precipitate.
  • the final eluant obtained from anion exchanger about 400 lit., was concentrated to obtain purified steviosides having 45.47% stevioside as the end product.
  • the soaking of dried plant material in minimum amount of water would have softened the plant tissue, which further facilitated easy extraction of steviosides when steam was directly injected in to the extractor.
  • the live steam surrendered its readily available latent heat onto the wet plant tissue, which helped in quick isolation of steviosides through the cell walls.
  • the directly injected steam create an agitation effect, which helps in instantaneous uniform heat distribution and cell wall rupture throughout the feed material whereby increasing the rate of extraction of steviosides.
  • the aqueous extract was partially purified by treating only with an alkali to remove various chelating, high molecular weight and colouring compounds in the form of a precipitate.
  • the filtrate separated from precipitate was directly subjected to various combinations of gel and macroporous type ion exchange resins. This not only cut-short the process purification time but also enabled the process to be carried out in an aqueous medium by avoiding intervention of organic solvents and also affecting the cost of production.
  • the main advantages of the present invention are: 1. The process is performed with safer and reusable chemicals like water, ion exchange resins in the food grade range and the entire process is carried out in only one solvent phase and that is water.
  • the extraction of the plant material is performed by directly injecting steam where the maximum steviosides are recovered in less time and in little water, which reduces the capital investment on plant machinery.
  • the separated filtrate is further purified by directly subjecting onto ion exchanger resins.
  • the process is simplified by eliminating usage of polymeric adsorbent resins and organic solvents.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Saccharide Compounds (AREA)
  • Seasonings (AREA)

Abstract

Procédé permettant de produire des stéviosides à partir de Stevia rebaudiana Bertoni, selon lequel on extrait le matériau végétal comminué en injectant directement de la vapeur dans l’extracteur, on filtre pour obtenir un extrait aqueux, et on traite par un alcali afin d’éliminer les composés non désirés sous la forme de précipités. L’extrait aqueux traité est filtré et le filtrat traité, d’abord au moyen d’une résine échangeuse de cations d’acide fort en gel ou macroporeuse, puis au moyen d’une résine échangeuse d’anions de base faible en gel ou macroporeuse. L’éluant aqueux contenant les stéviosides est concentré pour obtenir des stéviosides purifiés.
PCT/IN2004/000404 2004-10-04 2004-12-24 Procede de production de steviosides a partir de stevia rebaudiana bertoni Ceased WO2006038221A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN1914DE2004 2004-10-04
IN1914DEL2004 2004-10-04

Publications (1)

Publication Number Publication Date
WO2006038221A1 true WO2006038221A1 (fr) 2006-04-13

Family

ID=34960572

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IN2004/000404 Ceased WO2006038221A1 (fr) 2004-10-04 2004-12-24 Procede de production de steviosides a partir de stevia rebaudiana bertoni

Country Status (2)

Country Link
KR (1) KR100944242B1 (fr)
WO (1) WO2006038221A1 (fr)

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007149672A3 (fr) * 2006-06-19 2008-04-10 Coca Cola Co Composition de rebaudioside a et procédé de purification du rebaudioside a
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
US8030481B2 (en) 2007-05-21 2011-10-04 The Coca-Cola Company Stevioside polymorphic and amorphous forms, methods for their formulation, and uses
CN103304611A (zh) * 2013-06-18 2013-09-18 聊城大学 一种从瓜蒌皮中分离纯化3种黄酮苷的方法
EP2528455A4 (fr) * 2010-01-28 2013-11-27 Cargill Inc Procedes de traitement de melanges de glycosides pour obtenir un ou plusieurs de ces glycosides sous forme plus pure
CN103570778A (zh) * 2013-11-04 2014-02-12 西北大学 一种高纯度莱鲍迪甙a的制备方法
US8937168B2 (en) 2007-01-22 2015-01-20 Cargill, Incorporated Method of producing purified rebaudioside A compositions using solvent/antisolvent crystallization
US9012626B2 (en) 2006-06-19 2015-04-21 The Coca-Cola Company Rebaudioside a composition and method for purifying rebaudioside a
US20150141632A1 (en) * 2010-03-12 2015-05-21 Purecircle Usa Inc. High-purity steviol glycosides
US9131718B2 (en) 2009-06-16 2015-09-15 Epc (Beijing) Natural Products Co., Ltd. Process for rebaudioside D
CN105001281A (zh) * 2015-06-18 2015-10-28 晨光生物科技集团股份有限公司 一种同步生产甜菊糖苷、黄酮和绿原酸的工业化生产方法
CN105541937A (zh) * 2016-01-19 2016-05-04 苏州赛分科技有限公司 甜叶菊中甜菊糖苷的提取方法
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
US11414448B2 (en) 2010-11-19 2022-08-16 Cargill, Incorporated Method for the enrichment of rebaudioside b and/or rebaudioside d in stevia-derived glycoside compositions using adsorb-desorb chromatography with a macroporous neutral adsorbent resin
US11773125B2 (en) 2010-03-12 2023-10-03 Purecircle Usa Inc. Methods of preparing steviol glycosides and uses of the same
US12479877B2 (en) 2010-03-12 2025-11-25 The Coca-Cola Company Methods for purifying steviol glycosides and uses of the same

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5430199A (en) * 1977-08-08 1979-03-06 Sanyo Kokusaku Pulp Co Ltd Purification of stevia sweetening agnet
JPS54122300A (en) * 1978-03-14 1979-09-21 Teruaki Kushiken Purification of stevioside
JPS5581567A (en) * 1978-12-13 1980-06-19 Res Inst For Prod Dev Extraction and purification of stevioside
JPS575663A (en) * 1980-06-13 1982-01-12 Res Inst For Prod Dev Purification of stevioside through extraction
US4892938A (en) * 1987-07-21 1990-01-09 Giovanetto Roger H Method for the recovery of steviosides from plant raw material
RU1796128C (ru) * 1990-10-17 1993-02-23 Г.П.Сарджвеладзе и Л.Г.Харебава Способ получени концентрата из растени SтеVIа RеваUDIаNа ВеRтоNI
WO2000049895A1 (fr) * 1997-07-19 2000-08-31 National Research Council Of Canada EXTRACTION DE COMPOSES SUCRES A PARTIR DE $i(STEVIA REBAUDIANA BERTONI)

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5430199A (en) * 1977-08-08 1979-03-06 Sanyo Kokusaku Pulp Co Ltd Purification of stevia sweetening agnet
JPS54122300A (en) * 1978-03-14 1979-09-21 Teruaki Kushiken Purification of stevioside
JPS5581567A (en) * 1978-12-13 1980-06-19 Res Inst For Prod Dev Extraction and purification of stevioside
JPS575663A (en) * 1980-06-13 1982-01-12 Res Inst For Prod Dev Purification of stevioside through extraction
US4892938A (en) * 1987-07-21 1990-01-09 Giovanetto Roger H Method for the recovery of steviosides from plant raw material
RU1796128C (ru) * 1990-10-17 1993-02-23 Г.П.Сарджвеладзе и Л.Г.Харебава Способ получени концентрата из растени SтеVIа RеваUDIаNа ВеRтоNI
WO2000049895A1 (fr) * 1997-07-19 2000-08-31 National Research Council Of Canada EXTRACTION DE COMPOSES SUCRES A PARTIR DE $i(STEVIA REBAUDIANA BERTONI)

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
CHENG, T. F. ET AL: "Study on the purification of steviosides with the use of ion- exchange resins", ZHONGGUO NONGYE HUAXUE HUIZHI , 23(1-2), 178-90 CODEN: CKNHAA; ISSN: 0578-1736, 1985, XP009046787 *
DATABASE WPI Section Ch Week 199417, Derwent World Patents Index; AN 142958 *
DATABASE WPI Week 197944, Derwent World Patents Index; AN 79856B *
PATENT ABSTRACTS OF JAPAN vol. 003, no. 055 (C - 045) 11 May 1979 (1979-05-11) *
PATENT ABSTRACTS OF JAPAN vol. 004, no. 129 (C - 024) 10 September 1980 (1980-09-10) *
PATENT ABSTRACTS OF JAPAN vol. 006, no. 063 (C - 099) 22 April 1982 (1982-04-22) *

Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8791253B2 (en) 2006-06-19 2014-07-29 The Coca-Cola Company Rebaudioside A composition and method for purifying rebaudioside A
WO2007149672A3 (fr) * 2006-06-19 2008-04-10 Coca Cola Co Composition de rebaudioside a et procédé de purification du rebaudioside a
US9012626B2 (en) 2006-06-19 2015-04-21 The Coca-Cola Company Rebaudioside a composition and method for purifying rebaudioside a
US8937168B2 (en) 2007-01-22 2015-01-20 Cargill, Incorporated Method of producing purified rebaudioside A compositions using solvent/antisolvent crystallization
US8030481B2 (en) 2007-05-21 2011-10-04 The Coca-Cola Company Stevioside polymorphic and amorphous forms, methods for their formulation, and uses
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
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
EP2528455A4 (fr) * 2010-01-28 2013-11-27 Cargill Inc Procedes de traitement de melanges de glycosides pour obtenir un ou plusieurs de ces glycosides sous forme plus pure
US9562064B2 (en) * 2010-03-12 2017-02-07 Purecircle Sdn Bhd High-purity steviol glycosides
US20150141632A1 (en) * 2010-03-12 2015-05-21 Purecircle Usa Inc. High-purity steviol glycosides
US12479877B2 (en) 2010-03-12 2025-11-25 The Coca-Cola Company Methods for purifying steviol glycosides and uses of the same
US12037356B2 (en) 2010-03-12 2024-07-16 Purecircle Usa Inc. Methods of preparing steviol glycosides and uses of the same
US11773125B2 (en) 2010-03-12 2023-10-03 Purecircle Usa Inc. Methods of preparing steviol glycosides and uses of the same
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
US11414448B2 (en) 2010-11-19 2022-08-16 Cargill, Incorporated Method for the enrichment of rebaudioside b and/or rebaudioside d in stevia-derived glycoside compositions using adsorb-desorb chromatography with a macroporous neutral adsorbent resin
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
CN103304611A (zh) * 2013-06-18 2013-09-18 聊城大学 一种从瓜蒌皮中分离纯化3种黄酮苷的方法
CN103304611B (zh) * 2013-06-18 2016-06-15 山东中医药大学 一种从瓜蒌皮中分离纯化3种黄酮苷的方法
CN103570778B (zh) * 2013-11-04 2017-07-28 西北大学 一种高纯度莱鲍迪甙a的制备方法
CN103570778A (zh) * 2013-11-04 2014-02-12 西北大学 一种高纯度莱鲍迪甙a的制备方法
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
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
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
CN105001281B (zh) * 2015-06-18 2018-02-09 晨光生物科技集团股份有限公司 一种同步生产甜菊糖苷、黄酮和绿原酸的工业化生产方法
CN105001281A (zh) * 2015-06-18 2015-10-28 晨光生物科技集团股份有限公司 一种同步生产甜菊糖苷、黄酮和绿原酸的工业化生产方法
CN105541937B (zh) * 2016-01-19 2019-11-05 苏州赛分科技有限公司 甜叶菊中甜菊糖苷的分离纯化方法
CN105541937A (zh) * 2016-01-19 2016-05-04 苏州赛分科技有限公司 甜叶菊中甜菊糖苷的提取方法

Also Published As

Publication number Publication date
KR100944242B1 (ko) 2010-02-24
KR20080074020A (ko) 2008-08-12

Similar Documents

Publication Publication Date Title
US20060142555A1 (en) Process for production of steviosides from stevia rebaudiana bertoni
KR100944242B1 (ko) 스테비아 레바우디아나 베르토니로부터 스테비오사이드를생산하는 방법
CN101717418B (zh) 模拟移动床一步法分离甜叶菊甙技术
JPH0245637B2 (fr)
JPS62166861A (ja) ステビア乾葉からの甘味成分抽出・精製法
EP2315596B1 (fr) Procédé d'extraction de glucosinolates à partir de plantes
JPS62157B2 (fr)
CN108997359B (zh) 一种从甜菊糖生产废渣中提取叶绿素的方法
CN107325137A (zh) 一种甜菊糖苷的提取方法
CN110229201B (zh) 一种制备高纯度甜菊糖苷rm的工艺方法
CN111297936A (zh) 一种从罗汉果根中提取并分离总黄酮、总三萜皂苷和总多糖的方法
CN111793102A (zh) 从芷江野生甜茶中分离三叶苷和根皮苷的方法
CN109293791B (zh) 紫丁香蘑水溶性多糖及其制备方法与应用
CN113952367B (zh) 一种骨碎补提取物生产工艺
CN104788515B (zh) 一种减压超声辅助提取制备高纯度水溶性橄榄苦甙的方法
US7524526B2 (en) Process for producing high purity isoflavones
CN112225774A (zh) 一种高纯高提取率的新型茶皂素提取方法
CN100415697C (zh) 从油菜籽饼粕或油菜籽种皮中提取多酚的萃取剂及其制备方法
CN111349127A (zh) 一种甜菊糖苷的生产方法
CN116496328A (zh) 一种同时制备黄芩苷和汉黄芩苷的工艺方法
CN111747958B (zh) 一种从非洲马铃果中分离多种活性成分的方法
CN116600655A (zh) 用于纯化包含一种或多种甜菊糖苷的粗组合物的方法
CN115779006B (zh) 一种从猫爪草中提取并分离多糖、皂苷和有机酸的方法
CN114621305A (zh) 一种甜菊糖的提取和精制工艺
CN110156601A (zh) 一种从甜叶菊中制备高纯度绿原酸的方法

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BW BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE EG ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NA NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SM SY TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): BW GH GM KE LS MW MZ NA SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LT LU MC NL PL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

DPEN Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed from 20040101)
121 Ep: the epo has been informed by wipo that ep was designated in this application
NENP Non-entry into the national phase

Ref country code: DE

WWE Wipo information: entry into national phase

Ref document number: 1020077010295

Country of ref document: KR

WWE Wipo information: entry into national phase

Ref document number: 1200700962

Country of ref document: VN

122 Ep: pct application non-entry in european phase