CN107474153B - A method of total reducing sugar is prepared from useless offal - Google Patents
A method of total reducing sugar is prepared from useless offal Download PDFInfo
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- CN107474153B CN107474153B CN201710832097.6A CN201710832097A CN107474153B CN 107474153 B CN107474153 B CN 107474153B CN 201710832097 A CN201710832097 A CN 201710832097A CN 107474153 B CN107474153 B CN 107474153B
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- reducing sugar
- total reducing
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- extracting solution
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a kind of methods that total reducing sugar is prepared from useless offal.This method mainly includes extraction and purification technology.Wherein, ultrasonic technique is introduced during the extraction process, accelerates extraction rate and efficiency；It replaces ethanol water as Extraction solvent using distillation, improves extraction efficiency, reduce extraction cost；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 AB-8 macroreticular resin selectivity, decoloration, de- albumen process are combined into one, effectively solve the problems such as Sevage method filters hardly possible as caused by protein emulsifying, traditional column chromatography decoloration, de- albumen process are avoided, the decoloration of total reducing sugar is improved, takes off protein efficiency.The patented technology utilizes for useless comprehensive tobacco stems and provides new approach.
Description
Technical field
The invention belongs to tobacco processing and comprehensive utilization of waste technical fields, and in particular to preparation is total from useless offal
The technique of sugar.
Background technique
In tobacco leaf picking with process, the waste/hypo-tobacco leafs such as a large amount of offal and offal are generated.China is leaf tobacco production
Big country produces 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 the fields such as food, medicine and fine chemistry industry have a wide range of applications
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 being dissolved out, being needed together in total reducing sugar extraction containing other compositions such as pigment, albumen in offal
It is further purified.It there is no at present about the document report for preparing total reducing sugar from offal.
Water extraction and enzymatic isolation method etc. are the common methods that current total sugar extracts.Traditional water extraction method energy consumption is high, extracts
Time length, low efficiency, and further relate 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 etc. that there are solvent usages
Disadvantage；There are poor selectivity, total reducing sugars to lose the disadvantages of big for active carbon decoloring；Sevage method take off albumen there are protein emulsifying phenomenon,
The problems such as filtering is difficult and largely uses toxic organic solvents.In view of the foregoing, reasonable utilization is not yet received in useless time of China offal,
It is directly abandoned, results in waste of resources and environmental pollution.
Summary of the invention
The shock wave and jet stream that the present invention is generated using ultrasonic wave destroy membrane structure, improve the extraction efficiency of total reducing sugar；
And the technological means such as selective absorption effect and ethanol selectivity precipitating for being combined macroreticular resin, improve the purifying effect of total reducing sugar
Rate provides a kind of new method to prepare total reducing sugar from useless offal.
A kind of operating procedure preparing total reducing sugar from useless offal is as follows:
(1) ultrasonic extraction
(1.1) 75 105 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(1.2) ultrasonic extraction, filtering, takes supernatant, obtains total reducing sugar extracting solution；
(2) purification process
(2.1) macroreticular resin AB-8 is added into total reducing sugar extracting solution, handles 35 h, 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 separation is collected precipitating, is washed
Wash precipitating；24 h are freeze-dried, total reducing sugar powder is obtained；
The percent of decolourization of the total reducing sugar powder is greater than 71%, deproteinizing rate and is greater than 61%, total reducing sugar yield greater than 8.2%, total reducing sugar purity
Greater than 85%.
The technical solution further limited is as follows:
In step (1.2), it is ultrasonically treated condition: 100 W of ultrasonic power, 50 70 DEG C of temperature, extraction time 40 80
min。
In step (2.1), by mass volume ratio macroreticular resin: total reducing sugar extracting solution (W: V) is 1 g:20,40 mL, total
Sugared extracting solution adds macroreticular resin AB-8.
In step (2.2), 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 dehydrated alcohol of 4 times of volumes is added in total reducing sugar concentrate, alcohol analyses 12 h at 4 DEG C；It is centrifuged under the conditions of 2400 r/min of revolving speed
15 min are separated, precipitating is collected, washs precipitating with dehydrated alcohol.
In step (2.2), freeze-drying condition is 40 DEG C, 30 mmHg are freeze-dried 24 h.
Advantageous effects of the invention embody in the following areas:
1. introduce ultrasonic technique during the extraction process, using microwave energy increase medium movement velocity and penetration power, to
Improve the extraction rate and efficiency of total reducing sugar；Replace ethanol water as Extraction solvent using distilled water, improve extraction efficiency,
Reduce extraction cost；Extraction process is not related to the processing of acid or alkali, and method is more simple and environmentally-friendly；
2. being combined the characteristics such as AB-8 macroreticular resin selection absorption and ethyl alcohol selection sedimentation in purifying process and removing
The impurity such as albumen and pigment in total reducing sugar make total reducing sugar purity reach 85% or more；It eliminates Sevage method and takes off albumen process and tradition
Column chromatography decoloration, de- albumen process, solve Sevage method cause because of protein emulsifying difficult filtering, column chromatography low efficiency and at
The problems such as this is high improves total reducing sugar purification efficiency, reduces purifying cost.
Specific embodiment
In order to keep the purpose of the present invention, technical solution clearer, this hair is further illustrated below by way of specific embodiment
It is bright.
Embodiment 1
1, the extraction of total reducing sugar
(1.1) 90 mL distilled water are added into the 60 mesh offals that 3 g have been crushed in；
(1.2) extracts 60 min under the conditions of ultrasonic power is 100 W, temperature is 60 DEG C.Filtering, takes supernatant, obtains
Total reducing sugar extracting solution.
2, the purifying of total reducing sugar
(2.1) is to above-mentioned total reducing sugar extracting solution, by macroreticular resin: total reducing sugar extracting solution (W: V) is that 1g: 30 mL addition is big
Hole Resin A B-8, handles 4 h, and filtering obtains total reducing sugar filtered fluid.
(2.2) above-mentioned total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume by 70 DEG C, obtains total reducing sugar concentrate；Xiang Qi
The dehydrated 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 collect precipitating, used
Dehydrated alcohol washing precipitating；40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, total reducing sugar powder is obtained.Total reducing sugar percent of decolourization is
82.1%, deproteinizing rate 71.8%, total reducing sugar yield are 9.2%, the purity of total reducing sugar is 93%.
Embodiment 2
1, the extraction of total reducing sugar
(1.1) 105 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(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 extracting solution.
2, the purifying of total reducing sugar
(2.1) Xiang Shangshu total reducing sugar extracting solution, by macroreticular resin: total reducing sugar extracting solution (W: V) is that 1g: 20 mL addition is big
Hole Resin A B-8, handles 4 h, and filtering obtains total reducing sugar filtered fluid.
(2.2) above-mentioned total reducing sugar filtered fluid is concentrated at 70 DEG C the 1/5 of initial volume, obtains total reducing sugar concentrate；Xiang Qi
The dehydrated 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 collect precipitating, used
Dehydrated alcohol washing precipitating；40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, total reducing sugar powder is obtained.Total reducing sugar percent of decolourization is
78.3%, deproteinizing rate 74.2%, total reducing sugar yield are 8.8%, total reducing sugar purity is 90%.
Embodiment 3
1, the extraction of total reducing sugar
(1.1) 90 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(1.2) 40 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 70 DEG C.Filtering, takes supernatant, obtains always
Sugared extracting solution.
2, the purifying of total reducing sugar
(1.1) Xiang Shangshu total reducing sugar extracting solution, by macroreticular resin: total reducing sugar extracting solution (W: V) is that 1g: 40 mL add macropore
Resin A B-8, handles 5 h, and filtering obtains total reducing sugar filtered fluid.
(1.2) above-mentioned total reducing sugar filtered fluid is concentrated at 70 DEG C the 1/5 of initial volume, obtains total reducing sugar concentrate；Xiang Qi
The dehydrated 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 collect precipitating, used
Dehydrated alcohol washing precipitating；40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, total reducing sugar powder is obtained.Total reducing sugar percent of decolourization is
76.6%, deproteinizing rate 70.7%, total reducing sugar yield are 8.3%, total reducing sugar purity is 88%.
Embodiment 4
1, the extraction of total reducing sugar
(1.1) 75 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(1.2) 60 min are extracted under the conditions of ultrasonic power is 100 W, temperature is 50 DEG C.Filtering, takes supernatant, obtains always
Sugared extracting solution.
2, the purifying of total reducing sugar
(1.1) Xiang Shangshu total reducing sugar extracting solution, by macroreticular resin: total reducing sugar extracting solution (W: V) is that 1g: 30 mL addition is big
Hole Resin A B-8, handles 3 h, and filtering obtains total reducing sugar filtered fluid.
(1.2) above-mentioned total reducing sugar filtered fluid is concentrated at 70 DEG C the 1/5 of initial volume, obtains total reducing sugar concentrate；Xiang Qi
The dehydrated 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 collect precipitating, used
Dehydrated alcohol washing precipitating；40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, total reducing sugar powder is obtained.Total reducing sugar percent of decolourization is
79.7%, deproteinizing rate 67.6%, total reducing sugar yield are 8.2%, total reducing sugar purity is 87%.
Embodiment 5
1, the extraction of total reducing sugar
(1.1) 75 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(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 extracting solution.
2, the purifying of total reducing sugar
(1.1) Xiang Shangshu total reducing sugar extracting solution, by macroreticular resin: total reducing sugar extracting solution (W: V) is that 1g: 40 mL addition is big
Hole Resin A B-8, handles 3 h, and filtering obtains total reducing sugar filtered fluid.
(1.2) above-mentioned total reducing sugar filtered fluid is concentrated at 70 DEG C the 1/5 of initial volume, obtains total reducing sugar concentrate；Xiang Qi
The dehydrated 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 collect precipitating, used
Dehydrated alcohol washing precipitating；40 DEG C, 30 mmHg, 24 h of freeze-drying are deposited in, total reducing sugar powder is obtained.Total reducing sugar percent of decolourization is
71.8%, deproteinizing rate 61.5%, total reducing sugar yield are 8.2%, total reducing sugar purity is 85%.
Claims (1)
1. a kind of method for preparing total reducing sugar from useless offal, it is characterised in that following operating procedure:
(1) ultrasonic extraction
(1.1) 75 105 mL distilled water are added into the 60 mesh offals that 3 g have been crushed；
(1.2) ultrasonic extraction, filtering, takes supernatant, obtains total reducing sugar extracting solution；Ultrasonic treatment condition: 100 W of ultrasonic power, temperature
50 70 DEG C, 40 80 min of extraction time；
(2) purification process
(2.1) macroreticular resin AB-8 is added into total reducing sugar extracting solution, handles 35 h, filtering obtains total reducing sugar filtered fluid；By mass body
Product is than macroreticular resin AB-8: total reducing sugar extracting solution is 1 g:20,40 mL；
(2.2) total reducing sugar filtered fluid is concentrated into the 1/5 of initial volume at 70 DEG C, obtains total reducing sugar concentrate；Into total reducing sugar concentrate
The dehydrated alcohol of 4 times of volumes is added, alcohol analyses 12 h at 4 DEG C；15 min are centrifugated under the conditions of 2400 r/min of revolving speed,
Precipitating is collected, washs precipitating with dehydrated alcohol；24 h are freeze-dried, freeze-drying condition is 40 DEG C, 30 mmHg are freeze-dried
24 h obtain total reducing sugar powder；
The percent of decolourization of the total reducing sugar powder is greater than 71%, deproteinizing rate and is greater than greater than 61%, total reducing sugar yield greater than 8.2%, total reducing sugar purity
85%。
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| 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 (1)
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104725524B (en) * | 2015-03-31 | 2016-10-19 | 川渝中烟工业有限责任公司 | Utilize the method that homogenate extraction technology extracts Nicotiana tabacum L. polysaccharide from the waste tobacco stem of land for growing field crops |
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| 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 |
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