CN105503974A - Method for removing residual plasticizers from stevioside products - Google Patents

Method for removing residual plasticizers from stevioside products Download PDF

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Publication number
CN105503974A
CN105503974A CN201510981813.8A CN201510981813A CN105503974A CN 105503974 A CN105503974 A CN 105503974A CN 201510981813 A CN201510981813 A CN 201510981813A CN 105503974 A CN105503974 A CN 105503974A
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CN
China
Prior art keywords
stevioside
fluidizer
steviol glycoside
adsorption
macroporous adsorbent
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.)
Pending
Application number
CN201510981813.8A
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Chinese (zh)
Inventor
廖春龙
袁长荣
余桂春
谢芳
肖娟
胡启胜
郁军
李善汪
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PureCircle Jiangxi Biotechnology Co Ltd
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PureCircle Jiangxi Biotechnology Co Ltd
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Priority to CN201510981813.8A priority Critical patent/CN105503974A/en
Publication of CN105503974A publication Critical patent/CN105503974A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification

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  • 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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention relates to the field of agricultural chemistry and provides a method for removing residual plasticizers from stevioside products. A column type fixed-bed adsorption method is adopted, macro-porous adsorption resin is used as an adsorbent, a stevioside aqueous solution or an ethanol solution containing plasticizer residues passes through an adsorption column, and the residual plasticizers in the stevioside products are removed through adsorption. With the adoption of the method, through simple transformation of the stevioside production technology, the residual plasticizers in the stevioside products are removed through adsorption, and the removal rate can be up to 100%. The method is simple to operate, conditions are easy to control, and industrialization is easy. Stevioside after deep treatment with the method contains no plasticizers, and the method has the important significance in production and application of the stevioside.

Description

The minimizing technology of residual fluidizer in a kind of Stevioside products
Technical field
The present invention relates to agrochemical field, particularly the minimizing technology of residual fluidizer.
Background technology
Stevioside products is from catananche---a kind of high sugariness extracted the blade of sweet Stevia, low calorie, taste matter are good, the extraordinary a kind of novel pure natural sweeting agent of safety non-toxic, market outlook, can be widely used in the industries such as food, beverage, medicine, daily chemical industry.
Fluidizer (Plasticizer) is as the term suggests be exactly the additive of plastic cement.Add man-hour at plastic material, add fluidizer and its physical properties can be made to become comparatively softness, be easy to processing.According to the function used, environment difference, manufacture and have the soft durometer of various toughness, the finished product of gloss, the required fluidizer added of wherein softer plastic cement finished product the more.Fluidizer kind nearly over one hundred kind, but the compound for phthalate using the most general.
Phthalic ester is water white oily liquids mostly, generally be insoluble in water, be soluble in organic solvent, belong to middle polarity material, by breathing, diet and skin contact enter everybody and in animal body, thrombocyte in it and blood has very strong avidity, can be combined with each other and form small aggregate, thus cause thrombus.After acute suction people phthalic ester steam, respiratory tract and eye mucosa irritation symptom can be there is.Long-term skin contact phthalic ester there will be sensitization.It generally shows as middle minuent to the toxicity of humans and animals, is mainly manifested in 3 aspects: acute toxicity to the harm of population health; Carcinogenic, teratogenesis, mutagenesis; Reproductive and developmental toxicity.
In steviol glycoside production process, inevitably touch plastics, as pipeline, pad, diaphragm etc. and ethanol etc., so fluidizer remains uncontrollable in Stevioside products.
Solve the problem that product fluidizer is residual, have following methods at present: 1, the use of plastics in strict production control process, uses containing the pipeline, pad etc. of fluidizer, the strict content of plasticizing agent monitoring controlled in the auxiliary materials such as ethanol; 2, use gac to adsorb steviol glycoside feed liquid, remove fluidizer.
Above two kinds of methods have respective limitation, inevitably touch plastics in process of production, the production line particularly put into production, and change not containing the equipment part of fluidizer, spend huge, and effect is also difficult to ensure; Gac is used to carry out, except plasticizer treats, easily polluting production environment, being difficult to the requirement reaching cleaner production to steviol glycoside feed liquid.
Summary of the invention
Object of the present invention solves in steviol glycoside production process to exist and is difficult to avoid contacting plastics, and fluidizer is difficult to the problem of removal, the minimizing technology of residual fluidizer in a kind of Stevioside products is provided, just can be reached the effect well removing fluidizer by simple technique.
Technical problem of the present invention is solved mainly through following technical proposals:
Adopting pillar ADSORPTION IN A FIXED BED method, take macroporous adsorbent resin as sorbent material, fluidizer residual in Adsorption Stevioside products, and described macroporous adsorbent resin is containing nitrogenous, oxygen, the sulphur polar functionalities base such as ester group or amide-containing, cyano group, phenolic hydroxyl group.By the aqueous solution (C:1 ~ 30%) of steviol glycoside or ethanolic soln, (alcohol concn is 1 ~ 40%, steviol glycoside concentration is 1 ~ 30%) pass through this adsorption column according to 1 ~ 3BV/h flow velocity, make the fluidizer in steviol glycoside be adsorbed on macroporous adsorbent resin, effluent liquid is not containing fluidizer.
Carry out except plasticizer treats steviol glycoside with macroporous adsorbent resin, treatment capacity generally can reach the treatment capacity of 60 ~ 100kg/L, i.e. the steviol glycoside of 1L plastic resin treatment 60 ~ 100kg.
For ensureing that adsorption process is smooth and easy, the concentration of aqueous solution of above-mentioned steviol glycoside is C:1 ~ 30%, and excessive concentration easily blocks resin column; The ethanolic soln alcohol concn 1 ~ 40% of above-mentioned steviol glycoside, glycoside concentration is 1 ~ 30%.Flow velocity is that 1 ~ 3BV/h is advisable.
The physicochemical property of macroporous adsorbent resin are stablized, and can not have any impact in the process removing fluidizer on feed liquid.Macroporous adsorbent resin after using can carry out wash-out recovery with the ethanol of 40 ~ 60% concentration to the steviol glycoside in polymeric adsorbent, not containing fluidizer in the stevioside after recovery.
Reclaim the macroporous adsorbent resin after steviol glycoside to regenerate with the organic solvent of middle polarity or strong polarity, the fluidizer be adsorbed on polymeric adsorbent is eluted, reaches the object of regeneration.
The present invention is by the simple transformation to steviol glycoside production technique, and the fluidizer in Adsorption steviol glycoside, clearance can reach 100%.The present invention is easy and simple to handle, expense is low, be easy to industrialization.Steviol glycoside after the method advanced treatment, not containing fluidizer, has great importance in the production of steviol glycoside and application aspect.
Embodiment
Below technical scheme of the present invention is described in further detail.
Embodiment 1:
Before steviol glycoside feed liquid spraying dry, increase macroporous adsorptive resins, the feed liquid before spraying dry is carried out except plasticizer treats.
Before spray dry flow container, increase capacity is the resin container of 100L, and load the PC-A type macroporous adsorbent resin containing amide group, blade diameter length ratio is 1:5.The 20% steviol glycoside aqueous solution passes through this resin container with the speed of 100L/h.At process 40m 3stop charging after feed liquid, namely stop charging after 8MT steviol glycoside, treatment capacity is 80kg/L.To the steviol glycoside feed liquid sampling before and after charging, the third party feeler mechanism-Jiangxi Entry-Exit Inspection and Quarantine Bureau delivering to qualification is detected fluidizer common in steviol glycoside production process, and detected result is as follows:
Above data show, the steviol glycoside aqueous solution, after PC-A type middle polarity absorption with macroporous adsorbent resin, does not detect fluidizer and remains.
Embodiment 2:
Before steviol glycoside feed liquid removes alcohol, increase macroporous adsorptive resins, the feed liquid before spraying dry is carried out except plasticizer treats.
Before going alcohol operation, increase capacity is the resin container of 100L, and load the PC-B type macroporous adsorbent resin containing phenolic hydroxyl group, blade diameter length ratio is 1:5.5% steviol glycoside ethanolic soln (alcohol concn is 40%) passes through this resin container with the speed of 150L/h.At process 1200m 3stop charging after feed liquid, namely stop charging after 6MT steviol glycoside, treatment capacity is 60kg/L.To the steviol glycoside feed liquid sampling before and after charging, the third party feeler mechanism-Jiangxi Entry-Exit Inspection and Quarantine Bureau delivering to qualification is detected fluidizer common in steviol glycoside production process, and detected result is as follows:
Above data show, steviol glycoside ethanolic soln, after PC-B type absorption with macroporous adsorbent resin, does not detect fluidizer and remains.
The present embodiment is the embodiment of example of the present invention; for those skilled in the art; on the basis that the invention discloses application method and principle; be easy to make various types of improvement or distortion; and the structure be not limited only to described by the above-mentioned embodiment of the present invention, therefore previously described mode is preferred version, and does not have restrictive meaning; every equivalence done according to the present invention changes and amendment, all in the scope protection domain of claims of the present invention.

Claims (3)

1. in a Stevioside products, remain the minimizing technology of fluidizer, it is characterized in that, adopt pillar ADSORPTION IN A FIXED BED method, take macroporous adsorbent resin as sorbent material, fluidizer residual in Adsorption Stevioside products, described macroporous adsorbent resin is containing nitrogenous, oxygen, the sulphur polar functionalities base such as ester group or amide-containing, cyano group, phenolic hydroxyl group.
2. in a kind of Stevioside products according to claim 1, remain the minimizing technology of fluidizer, it is characterized in that: be the aqueous solution of steviol glycoside by the feed liquid of absorption with macroporous adsorbent resin post, its steviol glycoside concentration of the described aqueous solution is 1 ~ 30%, by 1 ~ 3BV/h flow velocity by this adsorption column.
3. in a kind of Stevioside products according to claim 1, remain the minimizing technology of fluidizer, it is characterized in that: be the ethanolic soln of steviol glycoside by the feed liquid of absorption with macroporous adsorbent resin post, its alcohol concn of described ethanolic soln is 1 ~ 40%, its steviol glycoside concentration is 1 ~ 30%, by 1 ~ 3BV/h flow velocity by this adsorption column.
CN201510981813.8A 2015-12-24 2015-12-24 Method for removing residual plasticizers from stevioside products Pending CN105503974A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510981813.8A CN105503974A (en) 2015-12-24 2015-12-24 Method for removing residual plasticizers from stevioside products

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510981813.8A CN105503974A (en) 2015-12-24 2015-12-24 Method for removing residual plasticizers from stevioside products

Publications (1)

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CN105503974A true CN105503974A (en) 2016-04-20

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107235949A (en) * 2017-06-16 2017-10-10 湖南华诚生物资源股份有限公司 A kind of extracting method without plasticiser cyanidin extract
CN111714953A (en) * 2020-06-18 2020-09-29 劲牌持正堂药业有限公司 Method for removing phthalate plasticizer in extract
CN112546665A (en) * 2020-12-01 2021-03-26 晨光生物科技集团股份有限公司 Method for removing plasticizer from pepper, preparation method of pepper oleoresin and pepper oleoresin
CN113956322A (en) * 2021-11-17 2022-01-21 湖南华诚生物资源股份有限公司 Method for removing harmful substances in momordica grosvenori extract

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杨扬: "《甜菊糖提取工艺进展及发展前景》", 《中国食品添加剂》 *
洪春苗: "《强碱性阴离子交换树脂降解去除水体中的PAEs》", 《持久性有机污染物论坛2011暨第六届持久性有机污染物全国学术研讨会论文集》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107235949A (en) * 2017-06-16 2017-10-10 湖南华诚生物资源股份有限公司 A kind of extracting method without plasticiser cyanidin extract
CN107235949B (en) * 2017-06-16 2020-06-05 湖南华诚生物资源股份有限公司 Method for extracting anthocyanin extract without plasticizer
CN111714953A (en) * 2020-06-18 2020-09-29 劲牌持正堂药业有限公司 Method for removing phthalate plasticizer in extract
CN112546665A (en) * 2020-12-01 2021-03-26 晨光生物科技集团股份有限公司 Method for removing plasticizer from pepper, preparation method of pepper oleoresin and pepper oleoresin
CN113956322A (en) * 2021-11-17 2022-01-21 湖南华诚生物资源股份有限公司 Method for removing harmful substances in momordica grosvenori extract

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Application publication date: 20160420