CN102924964B - Process for extracting and purifying monascus red pigment without citrinin - Google Patents
Process for extracting and purifying monascus red pigment without citrinin Download PDFInfo
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- CN102924964B CN102924964B CN201210409242.7A CN201210409242A CN102924964B CN 102924964 B CN102924964 B CN 102924964B CN 201210409242 A CN201210409242 A CN 201210409242A CN 102924964 B CN102924964 B CN 102924964B
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- monascorubin
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Abstract
The invention discloses a process for extracting and purifying a monascus red pigment without citrinin. The process for preparing the high-color-value and low-citrinin monascus red pigment comprises the following steps of: regulating a solution or fermentation liquor to a proper pH value which is 1.8 to 3.0 by using a hydrochloric acid at a proper concentration; settling the pigment to remove citrinin; and regulating the volume of ethanol, extraction time, pH value of an extraction solution, times of extraction, vacuum concentration temperature and vacuum degree. The method disclosed by the invention is easy to operate, reduces production cost and pigment loss (which is about 15% to 23%), and can effectively remove the citrinin in the pigment. The monascus red pigment prepared by the method has high color value and low citrinin and effectively expands the application range of monascus red pigment.
Description
Technical field
The present invention relates to one and do not produce extraction and purification process containing Citrinin monascorubin, especially utilize the aftertreatment technologys such as acidic treatment to remove the method for citrinin content in monascorubin product.
Background technology
Monascorubin, very extensive in the application of food service industry.But after French scientist doctor P.Blanc finds the kidney to have the Citrinin of carcinogenesis in monascorubin, the application of monascorubin is just subject to serious challenge in the international market.Therefore the Citrinin of removing or reduce in monascorubin is trend of the times, becomes the study hotspot of monascorubin industry in recent years.
Large quantity research shows that the generation of Citrinin and the production process of pigment are couplings, knocks out and the aspect such as strain improvement, the control of fermentation condition and the optimization of substratum both at home and abroad so far at the citrinin biosynthesis gene of removing research aspect Citrinin and reduction citrinin content and mainly concentrate on red colouring agent for food, also used as a Chinese medicine bacterial classification.Although also obtained certain effect, still have improved space, and, for the higher pigment product of this class citrinin content of Red kojic rice (powder), also do not reduce or remove at present the effective ways of Citrinin in pigment product.From pigment extraction purge process, the research of reduction or removal citrinin content is blank substantially.The present invention is further reduced or is removed the content of Citrinin in pigment product by the extraction and purification process taking acidic treatment as core after improveing, fill up the technological gap that reduces or remove Citrinin in last handling process, thereby provide strong technical guarantee for monascorubin application widely in food and other industry.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of monascorubin extraction and purification process that reduces or remove Citrinin.This extraction and purification process is based in the acidic solution that pH is lower, and Citrinin can fully be dissolved in the water, and most of monascorubin is precipitation state in state of saturation.By press filtration, the aqueous solution that contains Citrinin is separated, obtain the extremely low monascorubin that does not even contain Citrinin of citrinin content.
Technique provided by the present invention comprises the following steps:
1) pre-treatment of monascorubin liquid: by red kojic rice powder according to 1:10 ~ 20(m/m) ratio is fully dissolved in and in deionized water, makes solution, or the fermented liquid that finishes of deep layer liquid state fermentation;
2) solution of being prepared by step 1) or fermented liquid are adjusted pH value to 1.8 ~ 3.0 with strong acid hydrochloric acid, stir stir process 30 ~ 80min in adding hydrochloric acid soln;
3) by step 2) solution after treatment or fermented liquid get rid of after filtration waste liquid and leave filter residue;
4) step 3) is processed to gained filter residue according to solution or fermentating liquid volume 1:2 ~ 5(v/v before processing) with 70% alcohol extraction 2 ~ 4 times, after each extraction 3 ~ 5h, filter press obtains filtrate, while only extraction for the first time, adjusts pH to 6.5 ~ 7.4 with 40 ~ 60% caustic soda solns;
5) by step 4) gained filtrate after nanofiltration membrane is filtered, at 43 ~ 62 DEG C, vacuum tightness be to carry out vacuum concentration under-0.07 ~-0.1MPa condition, makes not the monascorubin concentrated solution that contains Citrinin, reclaims ethanol simultaneously;
6) by step 5) gained containing the spray-dried not monascorubin product containing Citrinin of making of the concentrated solution of ethanol.
For the citrinin content reducing to a greater extent in product reduces costs simultaneously, red kojic rice powder is according to 1:16(m/m) ratio is fully dissolved in deionized water and is advisable; Be that 1.8 ~ 3.0 stir process 45min are advisable by 55% hydrochloride adjusted solution or fermented liquid pH value; Add 1:2 ~ 5(v/v) 70% alcohol extraction 3 times, each 4.5h is advisable, and preferably extracting twice extracts 4.5h at every turn; Vacuum concentration is at 47 DEG C, and vacuum tightness is advisable under-0.095MPa condition.
The inventive method is simple to operate, and production cost is low, and pigment rate of loss low (being about 15% ~ 23%), can effectively remove the Citrinin in pigment product.It is high that monascorubin product prepared by the method has look valency,, containing the feature of Citrinin, do not improve monascorubin security, is the more wide world market of monascorubin developing.
Embodiment
Method in following embodiment, if no special instructions, is ordinary method.
Embodiment 1 utilizes red kojic rice powder to produce monascorubin treatment process
1) taking look valency is that the red kojic rice powder 30g of 2000u/g is fully dissolved in 500ml deionized water and makes solution, and sampling utilizes the serial HPLC of Agilent 1200 to detect citrinin content, and utilizes spectrophotometric determination look valency;
2) solution preparing is adjusted to pH value to 2.8 with 55% hydrochloric acid, while adding hydrochloric acid, slowly stir stir process 45min;
3) leave filter residue by getting rid of waste liquid after red colouring agent for food, also used as a Chinese medicine aqueous solution vacuum filtration after treatment;
4) whole gained filter residues are joined to 70% ethanol of 1200ml, equivalent 70% alcohol extraction 3 times, only 45% caustic soda soln adjusting pH to 6.9 for extraction for the first time, extracts 4.5h final vacuum suction filtration at every turn and obtains filtrate;
5) by gained filtrate after nanofiltration membrane is filtered, at 47 DEG C, vacuum tightness is carried out vacuum concentration under-0.095MPa condition, reclaims ethanol;
6) will not contain the spray-dried monascorubin product of making of concentrated solution of ethanol, utilize HPLC method to detect citrinin content, and utilize spectrophotometric determination look valency.
Carry out analyzing and testing according to look valency and citrinin content country examination criteria, detected result is: before processing, the total look valency of sample is 6000u, and citrinin content is 359mg/kg; After processing, total look valency is 4740u, does not detect Citrinin.Experimental result demonstration, pigment rate of loss is 21%, does not contain Citrinin in product.
Embodiment 2: liquid submerged fermentation method is produced monascorubin aftertreatment technology
The present invention requires not strict to fermented liquid, by general strategy, the fermented liquid that uses Monascus anka Nakazawa et sato fermentation to obtain all can meet requirement of the present invention.
1) use Monascus anka Nakazawa et sato, carry out deep layer liquid state fermentation taking rice as main raw material, after fermentation ends, collect fermented liquid, get liquid submerged fermentation and finish fermented liquid 500ml, sampling utilizes the serial HPLC of Agilent 1200 to detect citrinin content, and utilizes spectrophotometric determination look valency;
2) solution preparing is stirred to adjustment pH value to 2.8, stir process 45min with 55% the hydrochloric acid that slowly adds;
3) leave filter residue by getting rid of waste liquid after fermented liquid solution for vacuum suction filtration after treatment;
4) whole gained filter residues are joined to 70% ethanol of 1200ml, equivalent 70% alcohol extraction 3 times, only 45% caustic soda soln adjusting pH to 7.0 for extraction for the first time, extracts 4.5h final vacuum suction filtration at every turn and obtains filtrate;
5) by gained filtrate after nanofiltration membrane is filtered, at 47 DEG C, vacuum tightness is carried out vacuum concentration under-0.095MPa condition, reclaims ethanol;
6) will not contain the spray-dried monascorubin product of making of concentrated solution of ethanol, utilize HPLC method to detect citrinin content, and utilize spectrophotometric determination look valency.
Carry out analyzing and testing according to look valency and citrinin content country examination criteria, detected result is: before processing, the total look valency of sample is 162500u, and citrinin content is 24mg/L; After processing, total look valency is 133250u, does not detect Citrinin.Experimental result demonstration, pigment rate of loss is 18%, does not contain Citrinin in product.
Embodiment 3: plant size liquid submerged fermentation method is produced monascorubin aftertreatment technology
The present invention requires not strict to fermented liquid, by general strategy, the fermented liquid that uses Monascus anka Nakazawa et sato fermentation to obtain all can meet requirement of the present invention.
1) by 20m
3liquid submerged fermentation finishes to ferment liquid pump to stirred pot, and sampling utilizes the serial HPLC of Agilent 1200 to detect citrinin content, and utilizes spectrophotometric determination look valency;
2) adjust pH value to 2.8, stir process 45min to the hydrochloric acid that slowly adds 55% in stirred pot;
3) fermented liquid after treatment acid adjustment is utilized plate-and-frame filter press filter, get rid of waste liquid and leave filter residue;
4) whole gained filter residues be transferred to stirred pot and add 70% ethanol of 50t at every turn, extract 3 times, only 45% caustic soda soln adjusting pH to 7.0 for extraction for the first time, extract 4.5h at every turn after filter press obtain filtrate;
5) by gained filtrate after nanofiltration membrane is filtered, at 47 DEG C, vacuum tightness is carried out vacuum concentration under-0.095MPa condition, reclaims ethanol;
6) will not contain the spray-dried monascorubin product of making of concentrated solution of ethanol, utilize HPLC method to detect citrinin content, and utilize spectrophotometric determination look valency.
Carry out analyzing and testing according to look valency and citrinin content country examination criteria, detected result is: before processing, the total look valency of sample is 9.8 × 10
9u, citrinin content is 27mg/L; After processing, total look valency is 8.4 × 10
9u, does not detect Citrinin.Experimental result demonstration, pigment rate of loss is 15%, does not contain Citrinin in product.
Claims (2)
1. do not extract a purifying production process containing the monascorubin of Citrinin, it is characterized in that comprising the steps:
1) by red kojic rice powder according to 1:16(m/m) ratio is fully dissolved in and in deionized water, makes the red colouring agent for food, also used as a Chinese medicine aqueous solution, or Monascus anka Nakazawa et sato carries out deep layer liquid state fermentation taking rice as main raw material and finish the fermented liquid of mycetome;
2) add by stream while stirring the pH of mixed value that the mode of strong acid prepared step 1) slowly and be adjusted to 1.8～3.0, stir process 30～80min;
3) by step 2) mixed solution after treatment filters and gets rid of waste liquid and leave filter residue;
4) step 3) is processed to gained filter residue adds 2.5 times of volumes 70% ethanol according to filtration treatment front volume, equivalent 70% alcohol extraction 3 times, extract 4.5h at every turn after filter press obtain filtrate, while only extraction for the first time with 40～60% caustic soda solns adjust pH to 7.0;
5) by step 4) gained filtrate after nanofiltration membrane is filtered, at 47 DEG C, vacuum tightness is carried out vacuum concentration under-0.095MPa condition, makes the not monascorubin concentrated solution containing Citrinin, reclaims ethanol simultaneously;
6) by step 5) gained containing the spray-dried not monascorubin product containing Citrinin of making of the concentrated solution of ethanol;
Described step 2) in strong acid be hydrochloric acid, concentration is 30%-60%.
2. production technique according to claim 1, is characterized in that: the preferred filter press of described filtration.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103709781A (en) * | 2013-12-05 | 2014-04-09 | 南通双和食品有限公司 | Preparation method for natural haematochrome |
| CN104404084B (en) * | 2014-11-10 | 2015-11-18 | 广东科隆生物科技有限公司 | The monascorubin of a kind of monascorubin preparation method and acquisition thereof |
| CN104448919B (en) * | 2014-12-26 | 2016-06-01 | 天津商业大学 | The purification process of the pigment of hydroxyl |
| CN114836478A (en) * | 2022-04-22 | 2022-08-02 | 福州大学 | Method for extracting monascus red pigment with low citrinin |
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