CN107474153A - A kind of method that total reducing sugar is prepared from useless offal - Google Patents

A kind of method that total reducing sugar is prepared from useless offal Download PDF

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Publication number
CN107474153A
CN107474153A CN201710832097.6A CN201710832097A CN107474153A CN 107474153 A CN107474153 A CN 107474153A CN 201710832097 A CN201710832097 A CN 201710832097A CN 107474153 A CN107474153 A CN 107474153A
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China
Prior art keywords
reducing sugar
total reducing
extraction
useless
offal
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CN201710832097.6A
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CN107474153B (en
Inventor
洪深求
孙高军
周小兵
刘渊根
杨晓亮
张丽娜
郭建
尚静静
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ANHUI Co Ltd OF CHINA TOBACCO GENERAL Co Ltd
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ANHUI Co Ltd OF CHINA TOBACCO GENERAL Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

Abstract

The invention discloses a kind of method that total reducing sugar is prepared from useless offal.This method mainly includes extraction and purification technology.Wherein, ultrasonic technique is introduced in extraction process, accelerates extraction rate and efficiency;Ethanol water is replaced to improve extraction efficiency as Extraction solvent, reduce extraction cost by the use of distillation;The processing of acid or alkali it is not related in extraction process, method is more simple and environmentally-friendly.In purifying industry, utilize the adsorpting pigment and albumen of the macroreticular resins of AB 8 selectivity, it will decolourize, de- albumen process is combined into one, Sevage methods are effectively solved due to the problems such as filtering is difficult caused by protein emulsifying, avoid traditional column chromatography from decolourizing, de- albumen process, improve the decolouring of total reducing sugar, de- protein efficiency.The patented technology utilizes for useless comprehensive tobacco stems and provides new approach.

Description

A kind of method that total reducing sugar is prepared from useless offal
Technical field
The invention belongs to tobacco processing and waste's reclamation technical field, and in particular to be prepared from useless offal total The technique of sugar.
Background technology
In tobacco leaf harvesting with process, producing the waste/hypo-tobacco leafs such as substantial amounts of offal and offal.China is leaf tobacco production Big country, produce about 135 150 ten thousand tons of waste/hypo-tobacco leaf per year, wherein, nearly 80% is offal.Containing natural components such as polysaccharide in offal, have The multiple biological activities such as anti-oxidant, removing free radical, before being had a wide range of applications in fields such as food, medicine and fine chemistry industries Scape.
Offal is the thick and stiff vein part of tobacco leaf, and quality is hard, it is difficult to broken.Compared with offal, extracted from offal total The technical difficulty of sugar is big.In addition, also needed in offal containing other compositions such as pigment, albumen in total reducing sugar extraction by together dissolution It is further purified.The document report on preparing total reducing sugar from offal is there is no at present.
Water extraction and enzymatic isolation method etc. are the common methods of current its total sugar extraction.Traditional water extraction method high energy consumption, extraction Time is long, efficiency is low, and further relates to acid, alkali process;Although the enzymatic isolation method reaction time is short, can increase substantially total reducing sugar extraction Amount, but the price of enzyme is higher.Column chromatography is the common method of plant total reducing sugar purifying, big, time length of solvent load etc. be present Shortcoming;The shortcomings of poor selectivity, total reducing sugar loss is big be present in activated carbon decolorizing;Sevage methods take off albumen exist protein emulsifying phenomenon, The problems such as filtering is difficult and largely uses toxic organic solvents.In view of the foregoing, useless time of China offal is not yet rationally utilized, Directly it is abandoned, causes the wasting of resources and environmental pollution.
The content of the invention
The present invention destroys membrane structure using shock wave caused by ultrasonic wave and jet, improves the extraction efficiency of total reducing sugar; And the technological means such as selective absorption effect and the ethanol selectivity precipitation of macroreticular resin are combined with, improve the purifying effect of total reducing sugar Rate, a kind of new method is provided to prepare total reducing sugar from useless offal.
It is a kind of total reducing sugar is prepared from useless offal operating procedure it is as follows:
(1)Ultrasonic extraction
(1.1)75 105 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)Ultrasonic extraction, filtering, takes supernatant, obtains total reducing sugar extract solution;
(2)Purification process
(2.1)Macroreticular resin AB-8 is added into total reducing sugar extract solution, 35 h is handled, filtering, obtains total reducing sugar filtered fluid;
(2.2)Total reducing sugar filtered fluid is concentrated, obtains total reducing sugar concentrate;Alcohol analyses total reducing sugar concentrate;Centrifuge, collect precipitation, washing is heavy Form sediment;24 h are freeze-dried, obtain total reducing sugar powder;
The percent of decolourization of the total reducing sugar powder is more than 71%, deproteinizing rate and is more than more than 61%, total reducing sugar yield more than 8.2%, total reducing sugar purity 85%。
The technical scheme further limited is as follows:
Step(1.2)In, it is ultrasonically treated condition:The W of ultrasonic power 100,50 70 DEG C of temperature, the min of extraction time 40 80.
Step(2.1)In, by mass volume ratio macroreticular resin:Total reducing sugar extract solution(W :V)For 1 g:20 40 mL, total Sugared extract solution addition macroreticular resin AB-8.
Step(2.2)In, total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;To The absolute ethyl alcohol of 4 times of volumes is added in total reducing sugar concentrate, alcohol analyses 12 h at 4 DEG C;Centrifuged under the conditions of the r/min of rotating speed 2400 15 min are separated, precipitation is collected, precipitation is washed with absolute ethyl alcohol.
Step(2.2)In, freeze-drying condition is 40 DEG C, 30 mmHg are freeze-dried 24 h.
The advantageous effects of the present invention embody in the following areas:
1. ultrasonic technique is introduced in extraction process, using microwave energy increase medium movement velocity and penetration power, so as to improving The extraction rate and efficiency of total reducing sugar;Ethanol water is replaced to improve extraction efficiency as Extraction solvent, reduce by the use of distilled water Extraction cost;Extraction process is not related to the processing of acid or alkali, and method is more simple and environmentally-friendly;
2. in purifying process, it is combined with AB-8 macroreticular resins selection absorption and removes total reducing sugar with characteristics such as ethanol selection sedimentations In albumen and the impurity such as pigment, total reducing sugar purity is reached more than 85%;Eliminate Sevage methods and take off albumen process and conventional post color Spectrum is decolourized, de- albumen process, and solving Sevage methods causes that filtering is difficult, column chromatography efficiency is low and cost is high because of protein emulsifying The problems such as, total reducing sugar purification efficiency is improved, reduces purifying cost.
Specific embodiment
In order that the purpose of the present invention, technical scheme are clearer, this hair is further illustrated below by way of specific embodiment It is bright.
Embodiment 1
1st, the extraction of total reducing sugar
(1.1)90 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)60 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 60 DEG C.Filtering, takes supernatant, obtains total reducing sugar Extract solution.
2nd, the purifying of total reducing sugar
(2.1)To above-mentioned total reducing sugar extract solution, by macroreticular resin:Total reducing sugar extract solution(W :V)For 1g:30 mL add macropore tree Fat AB-8,4 h are handled, filtering, obtain total reducing sugar filtered fluid.
(2.2)Above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;Xiang Qi The absolute ethyl alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C;Then 15 min are centrifuged in 2400 r/min and collects precipitation, used Absolute ethyl alcohol washing precipitation;40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, obtain total reducing sugar powder.Total reducing sugar percent of decolourization is 82.1%th, deproteinizing rate 71.8%, total reducing sugar yield be 9.2%, the purity of total reducing sugar be 93%.
Embodiment 2
1st, the extraction of total reducing sugar
(1.1)105 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)80 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 60 DEG C.Filtering, takes supernatant, obtains total reducing sugar Extract solution.
2nd, the purifying of total reducing sugar
(2.1)To above-mentioned total reducing sugar extract solution, by macroreticular resin:Total reducing sugar extract solution(W :V)For 1g:20 mL add macropore tree Fat AB-8,4 h are handled, filtering, obtain total reducing sugar filtered fluid.
(2.2)Above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;Xiang Qi The absolute ethyl alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C;Then 15 min are centrifuged in 2400 r/min and collects precipitation, used Absolute ethyl alcohol washing precipitation;40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, obtain total reducing sugar powder.Total reducing sugar percent of decolourization is 78.3%th, deproteinizing rate 74.2%, total reducing sugar yield be 8.8%, total reducing sugar purity be 90%.
Embodiment 3
1st, the extraction of total reducing sugar
(1.1)90 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)40 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 70 DEG C.Filtering, takes supernatant, obtains total reducing sugar and carry Take liquid.
2nd, the purifying of total reducing sugar
(1.1)To above-mentioned total reducing sugar extract solution, by macroreticular resin:Total reducing sugar extract solution(W :V)For 1g:40 mL add macroreticular resin AB-8,5 h are handled, filtering, obtain total reducing sugar filtered fluid.
(1.2)Above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;Xiang Qi The absolute ethyl alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C;Then 15 min are centrifuged in 2400 r/min and collects precipitation, used Absolute ethyl alcohol washing precipitation;40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, obtain total reducing sugar powder.Total reducing sugar percent of decolourization is 76.6%th, deproteinizing rate 70.7%, total reducing sugar yield be 8.3%, total reducing sugar purity be 88%.
Embodiment 4
1st, the extraction of total reducing sugar
(1.1)75 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)60 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 50 DEG C.Filtering, takes supernatant, obtains total reducing sugar and carry Take liquid.
2nd, the purifying of total reducing sugar
(1.1)To above-mentioned total reducing sugar extract solution, by macroreticular resin:Total reducing sugar extract solution(W :V)For 1g:30 mL add macropore tree Fat AB-8,3 h are handled, filtering, obtain total reducing sugar filtered fluid.
(1.2)Above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;Xiang Qi The absolute ethyl alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C;Then 15 min are centrifuged in 2400 r/min and collects precipitation, used Absolute ethyl alcohol washing precipitation;40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, obtain total reducing sugar powder.Total reducing sugar percent of decolourization is 79.7%th, deproteinizing rate 67.6%, total reducing sugar yield be 8.2%, total reducing sugar purity be 87%.
Embodiment 5
1st, the extraction of total reducing sugar
(1.1)75 mL distilled water are added in the 60 mesh offals crushed to 3 g;
(1.2)80 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 60 DEG C.Filtering, takes supernatant, obtains total reducing sugar Extract solution.
2nd, the purifying of total reducing sugar
(1.1)To above-mentioned total reducing sugar extract solution, by macroreticular resin:Total reducing sugar extract solution(W :V)For 1g:40 mL add macropore tree Fat AB-8,3 h are handled, filtering, obtain total reducing sugar filtered fluid.
(1.2)Above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;Xiang Qi The absolute ethyl alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C;Then 15 min are centrifuged in 2400 r/min and collects precipitation, used Absolute ethyl alcohol washing precipitation;40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, obtain total reducing sugar powder.Total reducing sugar percent of decolourization is 71.8%th, deproteinizing rate 61.5%, total reducing sugar yield be 8.2%, total reducing sugar purity be 85%.

Claims (5)

  1. A kind of 1. method that total reducing sugar is prepared from useless offal, it is characterised in that following operating procedure:
    (1)Ultrasonic extraction
    (1.1)75 105 mL distilled water are added in the 60 mesh offals crushed to 3 g;
    (1.2)Ultrasonic extraction, filtering, takes supernatant, obtains total reducing sugar extract solution;
    (2)Purification process
    (2.1)Macroreticular resin AB-8 is added into total reducing sugar extract solution, 35 h is handled, filtering, obtains total reducing sugar filtered fluid;
    (2.2)Total reducing sugar filtered fluid is concentrated, obtains total reducing sugar concentrate;Alcohol analyses total reducing sugar concentrate;Centrifuge, collect precipitation, washing is heavy Form sediment;24 h are freeze-dried, obtain total reducing sugar powder;
    The percent of decolourization of the total reducing sugar powder is more than 71%, deproteinizing rate and is more than more than 61%, total reducing sugar yield more than 8.2%, total reducing sugar purity 85%。
  2. A kind of 2. method that total reducing sugar is prepared from useless offal according to claim 1, it is characterised in that:Step(1.2) In, it is ultrasonically treated condition:The W of ultrasonic power 100,50 70 DEG C of temperature, the min of extraction time 40 80.
  3. A kind of 3. method that total reducing sugar is prepared from useless offal according to claim 1, it is characterised in that:Step(2.1) In, by mass volume ratio macroreticular resin:Total reducing sugar extract solution(W :V)For 1 g:20 40 mL, macropore is added in total reducing sugar extract solution Resin A B-8.
  4. A kind of 4. method that total reducing sugar is prepared from useless offal according to claim 1, it is characterised in that:Step(2.2) In, total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate;4 are added into total reducing sugar concentrate The absolute ethyl alcohol of times volume, alcohol analyses 12 h at 4 DEG C;15 min are centrifuged under the conditions of the r/min of rotating speed 2400, it is heavy to collect Form sediment, precipitation is washed with absolute ethyl alcohol.
  5. A kind of 5. method that total reducing sugar is prepared from useless offal according to claim 1, it is characterised in that:Step(2.2) In, freeze-drying condition is 40 DEG C, 30 mmHg are freeze-dried 24 h.
CN201710832097.6A 2017-09-15 2017-09-15 A method of total reducing sugar is prepared from useless offal Expired - Fee Related CN107474153B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108325996A (en) * 2017-12-23 2018-07-27 佛山科学技术学院 A kind of method that abandoned biomass multi-direction synthetic utilizes

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3513857A (en) * 1967-12-26 1970-05-26 Philip Morris Inc Process for the treatment of tobacco stems
CN104725524A (en) * 2015-03-31 2015-06-24 川渝中烟工业有限责任公司 Method for extracting tobacco polysaccharides from waste tobacco stems in farmlands

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3513857A (en) * 1967-12-26 1970-05-26 Philip Morris Inc Process for the treatment of tobacco stems
CN104725524A (en) * 2015-03-31 2015-06-24 川渝中烟工业有限责任公司 Method for extracting tobacco polysaccharides from waste tobacco stems in farmlands

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘丹等: "大孔吸附树脂在天然产物分离纯化中的应用", 《中草药》 *
杨琛琛: "不同类型烟叶多糖的提取、结构及其性质研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108325996A (en) * 2017-12-23 2018-07-27 佛山科学技术学院 A kind of method that abandoned biomass multi-direction synthetic utilizes

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