CN101787385B - Preparation method for medical glucose with ultrahigh purity - Google Patents
Preparation method for medical glucose with ultrahigh purity Download PDFInfo
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- CN101787385B CN101787385B CN2010101206022A CN201010120602A CN101787385B CN 101787385 B CN101787385 B CN 101787385B CN 2010101206022 A CN2010101206022 A CN 2010101206022A CN 201010120602 A CN201010120602 A CN 201010120602A CN 101787385 B CN101787385 B CN 101787385B
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Abstract
The invention discloses a preparation method for medical glucose with ultrahigh purity. The steps of the method are as follows: (1) sweet potatoes or rice are soaked in water for 3 to 5 hours under room temperature and then pulped, and pulp liquid is filtered by an over 70-mesh filter screen; (2) the pH value of the pulp liquid is adjusted to 5.9 to 6.1, the mass concentration of the pulp liquid is adjusted to 29 to 33% after water is added, and then a calcium chloride assistant and high-temperature resistant amylase are added to the pulp liquid and are uniformly stirred with the pulp liquid;(3) the well-mixed pulp liquid is jetted and fluidized under the temperature of 109 to 115 DEG C, then cooled down to 90-95 DEG C and fluidized for 30-40 minutes; (4) a diatomite filter aid is added to the fluidized pulp liquid, and then the pulp liquid is filtered by plate-frame filtering equipment to remove components of proteins and fibers; (5) when filtering liquid is cooled down to 56-60 DEGC, the pH value of the pulp liquid is adjusted to 4.5-5.0, glucoamylase and debranching enzyme are added at the same time to saccharify the pulp liquid for 50-60 hours and are then killed to prepare the glucose; (6) the glucose is decolored and filtered; (7) ion exchange processing is carried out on the glucose; (8) the glucose is condensed; (9) the glucose is crystallized and dried; (10) the glucose is packed. The medical glucose prepared by the method of the invention contains no pyrotoxin substances, and the glucose content in the dry glucose can reach 99.5 to 99.7%.
Description
Technical field
The present invention relates to the preparation method of the medical glucose of a kind of ultra-high purity, especially relating to a kind of is the method that raw material is produced the medical glucose of ultra-high purity with sweet potato, rice.
Background technology
Dian Fentang mainly comprises SANMALT-S, isomeric maltose, glucose, high fructose syrup, maltodextrin, glucose and oligosaccharides (trisaccharide, tetrose etc.).Dian Fentang has that liquid is as clear as crystal, sweet taste soft pure, nutritious, calorific value is low, moisture retention is strong, Heat stability is good, characteristics such as edible not irritated; Be widely used in foodstuffs industry such as candy, cake, beverage, can, beer, cold drink, can also be used for light industry daily necessities industry and medicine and feedstuff industries etc. such as papermaking, toothpaste.Developed countries such as America and Europe are early than the deep development of just setting about Dian Fentang the fifties in last century, wherein with the U.S., the leading world of Japan and other countries Dian Fentang production technique.Glucose is one of Dian Fentang that present produced worldwide is historical for a long time, output is big, effect is wide.Glucose is the most a kind of monose of easy absorption of human body, and directly heat supply supplements the nutrients, and improves the systemic cell function, enhances metabolism, and has diuresis and detoxification, and its verivate also has important role to human body.Aspect medical, the glucose infusion liquid of 5-10% is widely used in the assisting therapy of various diseases; The hypertonic glucose liquid of 25-50% is mainly used in intravenous injection, is used for acute poisoning, bleeds too much, kidney property and cardiopulmonary property edema etc.With glucose, norfloxicin is that the norfloxicin glucose injection of raw material production is-kind of extensive pedigree antibiotic; Be mainly used in the treatment of the caused respiratory tract of susceptibility bacterium, urinary system, gastrointestinal tract infection clinically, good curative effect all arranged for ephritis, prostatitis, urocystitis, bronchitis, bacillary dysentery etc.In addition, research shows both at home and abroad at present, and glucose beverage can produce favorable influence to the man memory activity.Therefore, glucose and verivate thereof come into one's own day by day, become the focus product of domestic and international research and development and application, show its vast market prospect day by day in medicine, food and other fields.
Visible by the above, the purposes of glucose mainly is two aspects: food and pharmaceutical raw material.The glucose that is used for the food aspect is low relatively to hygienic requirements; Be used in the particularly glucose of injection aspect of medicine; Quite high to specification of quality; Not only require based on very high purity; And can not have the existence of any pyrotoxin, so-called pyrotoxin to cause the human body heating when being exactly pointed injection in the glucose or the general name of Hazardous substances such as feel cold, mainly be the intracellular toxin that harmful microorganism produces.
The method of producing glucose in history mainly contains two types: acid system and enzyme process.Before the eighties in 20th century, the whole world mainly is to adopt acid system to produce glucose.Along with the progress of science and technology, Production by Enzymes glucose rises gradually, and particularly 20 generation are since the nineties, and enzyme process replaces acid system fully.But the Production by Enzymes glucose with ultrahigh purity is appointed and is so also had a lot of technical bottleneck problems to have to be solved; At present; The production glucose with ultrahigh purity particularly major defect of the medical glucose of ultra-high purity is three aspects: the one, and can only be raw material production glucose generally at present with highly purified starch, production cost is higher; The 2nd, purity is difficult to surpass 99.5%; The 3rd, be easy to contaminating microorganisms (assorted bacterium) in the production process, cause pyrotoxin impurity such as intracellular toxin to exceed standard.
China is the largest production and the country of consumption of rice, produces about 1.9 hundred million tons of rice per year.The staple of rice is starch and protein, and wherein starch content accounts for about 80%.Have nearly 2,000 ten thousand tons of joints to crack rice and do not have fine utilization every year in the paddy processing (husk rice) simultaneously.In addition, sweet potato also is the large farm crop of China, is starch more than 75% in the dehydrated sweet potato material.Take by rice as the existing report of raw material production glucose, but in institute's malaga sugar, the content of glucose is lower, in its dry-matter, the content of glucose generally is difficult to surpass 90%.
Summary of the invention
The object of the present invention is to provide a kind of production cost low, do not contain pyrotoxin, is raw material with sweet potato or rice directly, and glucose content is higher than the preparation method of 99.5% the medical glucose of ultra-high purity in the product dry-matter.
The object of the invention is achieved through following technical scheme, and it may further comprise the steps:
(1) raw materials pretreatment: dried sweet potato (bar or bulk all can) or rice at room temperature were soaked in water 3-5 hour, and defibrination, slurries are crossed 70 orders with upper filter screen;
(2) size mixing: with hydrochloric acid or/and yellow soda ash adjustment slurry pH value to 5.9-6.1; Adding water, to adjust to mass concentration be 29-33% (or Baume concentration 17-19Be °); Add calcium chloride auxiliary agent and fire resistant alpha-diastase; The consumption of calcium chloride is dried sweet potato or the heavy 0.01-0.02% of rice, and the consumption of fire resistant alpha-diastase is dried sweet potato or the heavy 0.3-0.5% of rice, stirring and evenly mixing;
(3) high temperature liquefaction: the slurries that mix up at 109-115 ℃ of steam ejection liquefaction, were cooled to 90-95 ℃ in 5-20 minute, liquefied 30-40 minute, make liquefier;
(4) slag is taken off in filtration: in liquefier, add super-cell, diatomaceous consumption is dried sweet potato or the heavy 1-2wt% of rice raw material, filters through Plate Filtration equipment, takes off protein and fibre composition in the liquefier, and filtrating is used for next step saccharification;
(5) saccharification: the filtrating after to be filtered cools to 56-60 ℃, to 4.5-5.0, adds saccharifying enzyme and debranching factor with the hydrochloric acid adjust pH simultaneously; The consumption of saccharifying enzyme is dried sweet potato or the heavy 0.2-0.3wt% of rice, and the consumption of debranching factor is dried sweet potato or the heavy 0.08-0.10% of rice, saccharification time 50-60 hour; To saccharification liquid DE value (dextrose equivalent, i.e. dextrose equivalent value, vehicle economy value) >=98%; Be warming up to 85 ℃ of-90 ℃ of enzyme dischargings of going out with injector again, make saccharification liquid;
(6) decolorization filtering: in saccharification liquid, add the gac that is equivalent to dried sweet potato or the heavy 1-5wt% of rice raw material, stir, adjust pH is to 4.5-5.5; Under temperature 80-90 ℃; Filter through pressure filter, repeat press filtration 2-3 time of decolouring, as clear as crystal up to feed liquid; No carbon granule, foreign matter make the decolouring liquid glucose;
(7) ion exchange treatment: when the liquid glucose temperature of waiting to decolour drops to 50-55 ℃,, through anion-exchange resin column, carry out purifying again, make the liquid glucose of as clear as crystal free from extraneous odour, transparence >=95%, pH value 3.3-4.5 through cation exchange resin column;
(8) concentrate: will the liquid glucose after ion exchange resin treatment be concentrated to solid content with falling film evaporator and reach 72%-75%;
(9) crystallizing and drying: will concentrate liquid glucose and squeeze into clean crystallizer tank, and be cooled to 39-41 ℃ naturally, and be incubated 3-8 hour again, growing the grain, crystal seed continue decrease temperature crystalline after cultivating well, make the crystallization crystal even, and it is obvious that hand is pinched granular sensation, and discharging during to temperature 25-27 ℃ is centrifugal; Adopt the oven dry of hot gas flow drying system, control moisture content≤7wt%; It is dry to send into the cold air stream dehumidification system again, does not destroy to guarantee finished product glucose crystal, does not lump;
(10) packing.
Adopt the glucose of the inventive method preparation, the crystal grain rule, pure, free from extraneous odour.Detect by standard GB/regulation methods such as T 20880-2007, glucose content can reach 99.5-99.7% in its dry-matter.Detection is less than any pyrotoxin material.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
(1) dried sweet potato chip at room temperature was soaked in water 4 hours, defibrination, slurries are crossed 70 mesh filter screens;
(2)With hydrochloric acid or/and sodium carbonate solution adjustment slurry pH value to 6; Adding water adjustment mass concentration is 32%, adds calcium chloride auxiliary agent and fire resistant alpha-diastase, the consumption of calcium chloride be dried sweet potato heavy 0.01%; The consumption of fire resistant alpha-diastase be dried sweet potato heavy 0.4%, stirring and evenly mixing;
(3) with the slurries that mix up at 112 ℃ of steam ejection liquefactions, in 10 minutes, be cooled to 92 ℃, liquefied 35 minutes, make liquefier;
(4) in liquefier, add super-cell, diatomaceous consumption is the heavy 1.5wt% of dried sweet potato, filters through Plate Filtration equipment, takes off protein and fibre composition in the liquefier, and filtrating is used for next step saccharification;
(5) filtrating after to be filtered cools to 58 ℃, with hydrochloric acid adjust pH to 4.8, adds saccharifying enzyme and debranching factor simultaneously; The consumption of saccharifying enzyme is the heavy 0.25wt% of dried sweet potato; The consumption of debranching factor is that dried sweet potato weighs 0.09%, and saccharification time 55 hours is to saccharification liquid DE value >=98%; Be warming up to 88 ℃ of enzyme dischargings of going out with injector again, make saccharification liquid;
(6) decolorization filtering: in saccharification liquid, add the gac that is equivalent to the heavy 3wt% of dried sweet potato, stir, adjust pH to 5 under 85 ℃ of temperature, filters through pressure filter, press filtration 2 times that repeat to decolour, and as clear as crystal to feed liquid, no carbon granule, foreign matter make the decolouring liquid glucose;
(7) ion exchange treatment: when the liquid glucose temperature of waiting to decolour drops to 52 ℃,, through anion-exchange resin column, carry out purifying again, make the liquid glucose of as clear as crystal free from extraneous odour, transparence 95%, pH value 3.8 through cation exchange resin column;
(8) concentrate: will the liquid glucose after ion exchange resin treatment be concentrated to solid content with falling film evaporator and reach 73%;
(9) crystallizing and drying: will concentrate liquid glucose and squeeze into clean crystallizer tank, be cooled to 40 ℃ naturally, be incubated 6 hours again, growing the grain, crystal seed cultivate good after, the continuation decrease temperature crystalline makes the crystallization crystal even, it is obvious that hand is pinched granular sensation, discharging during to 26 ℃ of temperature is centrifugal; Adopt the oven dry of hot gas flow drying system, control moisture content 7wt%; It is dry to send into the cold air stream dehumidification system again, does not destroy to guarantee finished product glucose crystal, does not lump;
(10) packing.
The glucose of embodiment preparation, the crystal grain rule, pure, free from extraneous odour.Detect by standard GB/T 20880-2007 prescriptive procedure, glucose content reaches 99.6% in its dry-matter.Detection is less than any pyrotoxin material.
Embodiment 2
(1) raw materials pretreatment: rice at room temperature was soaked in water 3 hours, and defibrination, slurries are crossed 70 mesh filter screens;
(2) size mixing: with hydrochloric acid or/and yellow soda ash adjustment slurry pH value to 6.0; Adding water, to adjust to mass concentration be 30%, adds calcium chloride auxiliary agent and fire resistant alpha-diastase, the consumption of calcium chloride be rice heavy 0.012%; The consumption of fire resistant alpha-diastase be dried sweet potato or rice heavy 3%, stirring and evenly mixing;
(3) high temperature liquefaction: the slurries that mix up at 110 ℃ of steam ejection liquefactions, were cooled to 90 ℃ in 15 minutes, liquefied 40 minutes, make liquefier;
(4) slag is taken off in filtration: in liquefier, add super-cell, diatomaceous consumption is dried sweet potato or the heavy 1wt% of rice raw material, filters through Plate Filtration equipment, takes off protein and fibre composition in the liquefier, and filtrating is used for next step saccharification;
(5) saccharification: the filtrating after to be filtered cools to 56 ℃, with hydrochloric acid adjust pH to 4.5, adds saccharifying enzyme and debranching factor simultaneously; The consumption of saccharifying enzyme is the heavy 0.2wt% of rice; The consumption of debranching factor be rice heavy 0.10%, saccharification time 52 hours is to saccharification liquid DE value 98%; Be warming up to 90 ℃ of enzyme dischargings of going out with injector again, make saccharification liquid;
(6) decolorization filtering: in saccharification liquid, add the gac that is equivalent to the heavy 2wt% of rice, stir, adjust pH to 4.5 under 80 ℃ of temperature, filters through pressure filter, and press filtration 2 times that repeat to decolour make the decolouring liquid glucose;
(7) ion exchange treatment: when the liquid glucose temperature of waiting to decolour drops to 54 ℃,, through anion-exchange resin column, carry out purifying again, make the liquid glucose of as clear as crystal free from extraneous odour, transparence 97%, pH value 3.5 through cation exchange resin column;
(8) concentrate: will the liquid glucose after ion exchange resin treatment be concentrated to solid content with falling film evaporator and reach 74%;
(9) crystallizing and drying: will concentrate liquid glucose and squeeze into clean crystallizer tank, be cooled to 39 ℃ naturally, be incubated 7 hours again, growing the grain, crystal seed cultivate good after, the continuation decrease temperature crystalline makes the crystallization crystal even, it is obvious that hand is pinched granular sensation, discharging during to 26 ℃ of temperature is centrifugal; Adopt the oven dry of hot gas flow drying system, control moisture content 6wt%; It is dry to send into the cold air stream dehumidification system again, does not destroy to guarantee finished product glucose crystal, does not lump;
(10) packing.
The glucose of present embodiment preparation, the crystal grain rule, pure, free from extraneous odour.Detect by standard GB/regulation methods such as T 20880-2007, glucose content reaches 99.7% in its dry-matter.Detection is less than any pyrotoxin material.
Embodiment 3
(1) raw materials pretreatment: dried sweet potato piece at room temperature was soaked in water 3 hours, and defibrination, slurries are crossed 70 mesh filter screens;
(2)Size mixing: or/and yellow soda ash adjustment slurry pH value to 6.0, adding water, to adjust to mass concentration be 18Be ° of Baume concentration, adds calcium chloride auxiliary agent and fire resistant alpha-diastase with hydrochloric acid; The consumption of calcium chloride be dried sweet potato heavy 0.01%; The consumption of fire resistant alpha-diastase be dried sweet potato heavy 0.5%, stir mixing;
(3) high temperature liquefaction: the slurries that mix up at 110 ℃ of steam ejection liquefactions, were cooled to 90 ℃ in 20 minutes, liquefied 40 minutes, make liquefier;
(4) slag is taken off in filtration: in liquefier, add super-cell, diatomaceous consumption is the heavy 2wt% of dried sweet potato, filters through Plate Filtration equipment, takes off protein and fibre composition in the liquefier, and filtrating is used for next step saccharification;
(5) saccharification: the filtrating after to be filtered cools to 60 ℃, with hydrochloric acid adjust pH to 5.0, adds saccharifying enzyme and debranching factor simultaneously; The consumption of saccharifying enzyme is the heavy 0.3wt% of dried sweet potato; The consumption of debranching factor be dried sweet potato or rice heavy 0.08%, saccharification time 50 hours is to saccharification liquid DE value >=98%; Be warming up to 85 ℃ of ℃ of enzyme dischargings of going out with injector again, make saccharification liquid;
(6) decolorization filtering: in saccharification liquid, add the gac that is equivalent to the heavy 4wt% of dried sweet potato, stir, adjust pH to 4.5 under 80 ℃ of temperature, filters through pressure filter, press filtration 3 times that repeat to decolour, and as clear as crystal up to feed liquid, no carbon granule, foreign matter make the decolouring liquid glucose;
(7) ion exchange treatment: when the liquid glucose temperature of waiting to decolour drops to 50 ℃,, through anion-exchange resin column, carry out purifying again, make the liquid glucose of as clear as crystal free from extraneous odour, transparence 95%, pH value 3.5 through cation exchange resin column;
(8) concentrate: will the liquid glucose after ion exchange resin treatment be concentrated to solid content with falling film evaporator and reach 72%;
(9) crystallizing and drying: will concentrate liquid glucose and squeeze into clean crystallizer tank, be cooled to 41 ℃ naturally, be incubated 5 hours again, growing the grain, crystal seed cultivate good after, the continuation decrease temperature crystalline makes the crystallization crystal even, it is obvious that hand is pinched granular sensation, discharging during to 27 ℃ of temperature is centrifugal; Adopt the oven dry of hot gas flow drying system, control moisture content 7wt%; It is dry to send into the cold air stream dehumidification system again, does not destroy to guarantee finished product glucose crystal, does not lump;
(10) packing.
The glucose of present embodiment preparation, the crystal grain rule, pure, free from extraneous odour.Detect by standard GB/regulation methods such as T 20880-2007, glucose content reaches 99.6% in its dry-matter.Detection is less than any pyrotoxin material.
Claims (1)
1. the preparation method of a medical glucose with ultrahigh purity is characterized in that, may further comprise the steps:
(1) raw materials pretreatment: dried sweet potato or rice at room temperature were soaked in water 3-5 hour, and defibrination, slurries are crossed 70 orders with upper filter screen;
(2) size mixing: with hydrochloric acid or/and yellow soda ash adjustment slurry pH value to 5.9-6.1; Adding water, to adjust to mass concentration be 29-33%; Add calcium chloride auxiliary agent and fire resistant alpha-diastase; The consumption of calcium chloride is dried sweet potato or the heavy 0.01-0.02% of rice, and the consumption of fire resistant alpha-diastase is dried sweet potato or the heavy 0.3-0.5% of rice, stirring and evenly mixing;
(3) high temperature liquefaction: the slurries that mix up at 109-115 ℃ of steam ejection liquefaction, were cooled to 90-95 ℃ in 5-20 minute, liquefied 30-40 minute, make liquefier;
(4) slag is taken off in filtration: in liquefier, add super-cell, diatomaceous consumption is dried sweet potato or the heavy 1-2wt% of rice raw material, filters through Plate Filtration equipment, takes off protein and fibre composition in the liquefier, and filtrating is used for next step saccharification;
(5) saccharification: the filtrating after to be filtered cools to 56-60 ℃, to 4.5-5.0, adds saccharifying enzyme and debranching factor with the hydrochloric acid adjust pH simultaneously; The consumption of saccharifying enzyme is dried sweet potato or the heavy 0.2-0.3wt% of rice; The consumption of debranching factor is dried sweet potato or the heavy 0.08-0.10% of rice, saccharification time 50-60 hour, to saccharification liquid dextrose equivalent value >=98%; Be warming up to 85 ℃ of-90 ℃ of enzyme dischargings of going out with injector again, make saccharification liquid;
(6) decolorization filtering: in saccharification liquid, add the gac that is equivalent to dried sweet potato or the heavy 1-5wt% of rice raw material, stir, adjust pH is to 4.5-5.5; Under temperature 80-90 ℃; Filter through pressure filter, repeat press filtration 2-3 time of decolouring, as clear as crystal up to feed liquid; No carbon granule, foreign matter make the decolouring liquid glucose;
(7) ion exchange treatment: when the liquid glucose temperature of waiting to decolour drops to 50-55 ℃,, through anion-exchange resin column, carry out purifying again, make the liquid glucose of as clear as crystal free from extraneous odour, transparence >=95%, pH value 3.3-4.5 through cation exchange resin column;
(8) concentrate: will the liquid glucose after ion exchange resin treatment be concentrated to solid content with falling film evaporator and reach 72%-75%;
(9) crystallizing and drying: will concentrate liquid glucose and squeeze into clean crystallizer tank, and be cooled to 39-41 ℃ naturally, and be incubated 3-8 hour again, growing the grain, crystal seed continue decrease temperature crystalline after cultivating well, make the crystallization crystal even, and it is obvious that hand is pinched granular sensation, and discharging during to temperature 25-27 ℃ is centrifugal; Adopt the oven dry of hot gas flow drying system, control moisture content≤7wt%; It is dry to send into the cold air stream dehumidification system again, does not destroy to guarantee finished product glucose crystal, does not lump;
(10) packing.
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| CN102337316B (en) * | 2011-09-30 | 2013-07-31 | 广州双桥股份有限公司 | Process for producing starch sugar |
| CN102392009A (en) * | 2011-11-28 | 2012-03-28 | 上海景峰制药有限公司 | Method for purifying papain |
| CN102559811B (en) * | 2012-03-15 | 2013-04-17 | 吴允山 | Method of preparing sugar by utilizing sweet potato residues |
| CN103525887B (en) * | 2013-10-21 | 2015-09-09 | 诸城东晓生物科技有限公司 | A kind of crystalline dextrose production method of energy-conserving and environment-protective |
| CN108251569A (en) * | 2018-01-23 | 2018-07-06 | 山东兆光色谱分离技术有限公司 | A kind of DEXTROSE ANHYDROUS preparation process |
| CN111500794A (en) * | 2020-04-15 | 2020-08-07 | 潍坊盛泰药业有限公司 | Production method of water-containing glucose |
| CN112481419A (en) * | 2020-12-24 | 2021-03-12 | 山东辛仁生物科技有限公司 | Starch sugar solution refining method |
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| CN101608197A (en) * | 2009-07-27 | 2009-12-23 | 中南林业科技大学 | With rice is the method that raw material is produced oligomeric isomeric maltose |
| CN101608196A (en) * | 2009-07-27 | 2009-12-23 | 中南林业科技大学 | With rice is the method that raw material is produced high-purity maltose syrup |
| CN101613729A (en) * | 2009-07-27 | 2009-12-30 | 中南林业科技大学 | With rice is the method that raw material is produced low DE value maltodextrin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101608197A (en) * | 2009-07-27 | 2009-12-23 | 中南林业科技大学 | With rice is the method that raw material is produced oligomeric isomeric maltose |
| CN101608196A (en) * | 2009-07-27 | 2009-12-23 | 中南林业科技大学 | With rice is the method that raw material is produced high-purity maltose syrup |
| CN101613729A (en) * | 2009-07-27 | 2009-12-30 | 中南林业科技大学 | With rice is the method that raw material is produced low DE value maltodextrin |
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