CN101613419A - The method of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata - Google Patents
The method of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata Download PDFInfo
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Abstract
A kind of method of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata, dried fragrant plant mentioned in ancient texts water is floated impurity elimination, air-dry, pulverizing, handle with alcohol degreasing, HCI solution leaching, again through ultrasonic extraction, centrifugal filtrate, filtrate adds the NaOH neutralization, centrifugal with supernatant concentration, add ethanol and leave standstill, centrifugation, use the washing with alcohol throw out, drying under reduced pressure gets Sulfate of polysaccharide crude product A, and Crude polysaccharides A is mixed with the aqueous solution, adds ethanol, precipitate algin B, centrifugal, supernatant liquor add ethanol centrifugal again, the precipitation embathe with ethanol and acetone, the drying, Sulfate of polysaccharide C.The present invention adopts ultrasonic wave auxiliary heat acid system to extract Sulfate of polysaccharide from fragrant plant mentioned in ancient texts in conjunction with hot water, ultrasonic wave and acid system advantage, and the Sulfate of polysaccharide amount of extraction is bigger, and features simple and practical process, the less investment that needs in the production, and instant effect, technology is fit to extensively promote.
Description
Technical field
The invention belongs to the method for chemical industry field of food, particularly a kind of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata.
Background technology
Polysaccharide compound all has extensive existence in nature higher plant, algae, bacterium class and animal body, be the important composition composition of living matter.It not only can be controlled cell fission, also have a vital role of regulating the cell growth and the aspects such as organism eubolism that earn a bare living.Since the sixties, researchist's concern and attention more and more have been subjected to about STUDY ON POLYSACHAROSE.
/ 3rd of a ball total area is taken up an area of in the ocean, is containing extremely abundant Biological resources, is organic largest production person.Marine alga is the important component part of Living marine resources, is the natural enrichment person (comprising halogens such as chlorine, bromine, iodine) of the organic original producer and inorganics in the ocean.Contain abundant polysaccharide in the marine alga, account for the over half of marine alga dry weight, Sulfate of polysaccharide pair cell wherein has immunoregulation effect, antitumor action, antimutagenic effect, inducing cell differentiation, multiple efficacies such as antiviral.Widespread use and people's going deep into along with marine alga to the important living matter understanding of this class of Sulfate of polysaccharide, bioactive research more and more comes into one's own to Sulfate of polysaccharide, its extraction preparation and be applied to focus into industry research such as biology, medicine, food.
Fragrant plant mentioned in ancient texts belongs to rhodophyta, true Rhodophyceae, Gigartinales, fragrant plant mentioned in ancient texts section, Gracilaria, is the tropical marine alga, has at the South Sea of China widely to distribute.Fragrant plant mentioned in ancient texts not only grows soon, the output height, and economic worth is also very remarkable.Domestic research to fragrant plant mentioned in ancient texts mainly concentrates on the physico-chemical property of various fragrant plant mentioned in ancient texts agar and is subjected to seasonal variation and several respects such as the composition of the classification of the influence of different generations, agar, each fraction and chemical structure thereof, but the extraction preparation research to its Sulfate of polysaccharide is less, and concentrate on methods such as hot water and ultrasonic wave, and make alginic acid under low pH, be difficult to dissolving with the extraction of hot acid liquid, also can increase the extraction yield of Sulfate of polysaccharide.
Summary of the invention
The method that the purpose of this invention is to provide a kind of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata, sulfate content are 8.00～12.00%.Determined that by orthogonal test the hydrolysis appropriate processing condition is that concentration of hydrochloric acid 0.20%, material ratio 1: 40, extraction time are 65 ℃ of 25min and temperature.Make the polysaccharide sample by optimum extraction condition, polysaccharide content average out to 21.71%, sulfate content average out to 10.23%, protein content average out to 0.76%, the Gracilaria gigas Harvey polysaccharides sulfuric ester is the nonreducing sugar that a class contains sulfate group, the mixed polysaccharide of no starch and non-polyphenols.
The present invention floats impurity elimination with dried fragrant plant mentioned in ancient texts water, air-dry, pulverize, 85～95% alcohol degreasings are handled 2～3h, and material ratio 1: 40～1: 60 leaches with 60 ℃ HCI, 0.10～0.20% solution, power 500W ultrasonic extraction, centrifugal filtrate, filtrate adds NaOH and is neutralized to pH=7, and is centrifugal with supernatant concentration, add ethanol to 60～65%, leave standstill, the washing with alcohol throw out is used in centrifugation, drying under reduced pressure gets Sulfate of polysaccharide crude product A, Crude polysaccharides A is mixed with the aqueous solution, adds ethanol to 20～25%, precipitate algin B, centrifugal, supernatant liquor adds ethanol to 60～65%, centrifugal again, precipitation is embathed with ethanol and acetone, and 40～45 ℃ of dryings get Sulfate of polysaccharide C.
The present invention adopts ultrasonic wave auxiliary heat acid system to extract Sulfate of polysaccharide from fragrant plant mentioned in ancient texts in conjunction with hot water, ultrasonic wave and acid system advantage, and the Sulfate of polysaccharide amount of extraction is bigger, and features simple and practical process, the less investment that needs in the production, and instant effect, technology is fit to extensively promote.
Embodiment
The Sulfate of polysaccharide pair cell has immunoregulation effect, antitumor action, antimutagenic effect, inducing cell differentiation, multiple efficacies such as antiviral, its extraction preparation and be applied in industries such as biology, medicine, food and more and more come into one's own.Fragrant plant mentioned in ancient texts is the tropical marine alga, has at the South Sea of China widely to distribute.Fragrant plant mentioned in ancient texts not only grows soon, the output height, and economic worth is also very remarkable.This invention is to be that raw material therefrom extracts valuable Sulfate of polysaccharide material with the fragrant plant mentioned in ancient texts, for the comprehensive utilization of fragrant plant mentioned in ancient texts provides a kind of feasible method.
Determined that by orthogonal test the hydrolysis appropriate processing condition is that concentration of hydrochloric acid 0.20%, material ratio 1: 40, extraction time are 65 ℃ of 25min and temperature.(table 1,2).
Table 1 orthogonal experiment level of factor table
Table 2 orthogonal experiment scheme and interpretation of result
The present invention has measured the physico-chemical property of polysaccharide.The physico-chemical property of the Crude polysaccharides that obtains by optimum process condition, algin, Sulfate of polysaccharide sees Table 3.The protein content of three kinds of polysaccharide is very low, minimum with C, the Molish reaction, Feling reaction, IKI reaction, the ferric chloride reaction that only are 0.21%, three kind of sulfated polysaccharide are all negative, illustrate that they all do not contain reducing sugar, starch, polyphenols.
Table 3 Gracilaria gigas Harvey polysaccharides product physico-chemical property table
Embodiment 1
Starting material are handled:
Dried fragrant plant mentioned in ancient texts dish water floats impurity elimination, air-dry.Pulverize 85～95% ethanol and isopyknic petroleum ether degreasing and handle 2h, supernatant liquor reclaims ethanol, and the residue drying is used to extract polysaccharide.
Embodiment 2
Polysaccharide extracts flow process:
Dried fragrant plant mentioned in ancient texts water floats impurity elimination, air-dry, pulverizing, and 85～95% alcohol degreasings are handled 2～3h, material ratio 1: 40～1: 60, leach with 60 ℃ HCI, 0.10～0.20% solution, power 500W ultrasonic extraction, centrifugal filtrate, filtrate adds NaOH and is neutralized to pH=7, centrifugal with supernatant concentration, add ethanol to 60～65%, leave standstill, centrifugation, use the washing with alcohol throw out, drying under reduced pressure gets Sulfate of polysaccharide crude product A.
Crude polysaccharides A is mixed with the aqueous solution, adds ethanol to 20～25%, precipitate algin B, centrifugal, supernatant liquor adds ethanol to 60～65%, centrifugal, precipitation is embathed with ethanol and acetone again, 40～45 ℃ dry must Sulfate of polysaccharide C.
Embodiment 3
The mensuration of specific conductivity:
Polysaccharide soln concentration is 1 (mg/ml), is blank with distilled water, in 20 ℃ of mensuration.
Embodiment 4
The polysaccharide properties of samples is measured:
The evaluation of reducing sugar: Molish reaction, Fehling reaction; Starch is identified: the IKI reaction; Polyphenols is identified: ferric chloride reaction; Proteinic qualitative evaluation: ninhydrin reaction; The qualitative evaluation of sulfate: bariumchloride--gelatin reaction.
Claims (1)
1, a kind of method of ultrasonic acid extraction of sulfated polysaccharide from gracilaria tenuistipitata, it is characterized in that dried fragrant plant mentioned in ancient texts water is floated impurity elimination, air-dry, pulverize, 85～95% alcohol degreasings are handled 2～3h, material ratio 1: 40～1: 60, with 60 ℃ HCI, 0.10～0.20% solution leaching, power 500W ultrasonic extraction, centrifugal filtrate, filtrate adds NaOH and is neutralized to pH=7, centrifugal with supernatant concentration, add ethanol to 60～65%, leave standstill, centrifugation, use the washing with alcohol throw out, drying under reduced pressure gets Sulfate of polysaccharide crude product A, and Crude polysaccharides A is mixed with the aqueous solution, add ethanol to 20～25%, precipitate algin B, centrifugal, supernatant liquor adds ethanol to 60～65%, centrifugal again, precipitation is embathed with ethanol and acetone, 40～45 ℃ of dry Sulfate of polysaccharide C that get, sulfate content is 8.00～12.00%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266357A (en) * | 2010-06-01 | 2011-12-07 | 朱益生 | Method for improving antioxidant component content in asparagus schoberioides kunth extract |
| CN103704275A (en) * | 2013-12-10 | 2014-04-09 | 淮海工学院 | Separation and purification method and application for algae phenolic acids |
| CN109593140A (en) * | 2018-12-29 | 2019-04-09 | 广州暨南生物医药研究开发基地有限公司 | A kind of crispy gracilaria polysaccharide and its preparation method and application |
| CN115746160A (en) * | 2022-11-30 | 2023-03-07 | 南方海洋科学与工程广东省实验室(广州) | Method for reducing viscosity of polysaccharide |
-
2008
- 2008-06-23 CN CN200810029075A patent/CN101613419A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266357A (en) * | 2010-06-01 | 2011-12-07 | 朱益生 | Method for improving antioxidant component content in asparagus schoberioides kunth extract |
| CN102266357B (en) * | 2010-06-01 | 2012-11-21 | 朱益生 | Method for improving antioxidant component content in asparagus schoberioides kunth extract |
| CN103704275A (en) * | 2013-12-10 | 2014-04-09 | 淮海工学院 | Separation and purification method and application for algae phenolic acids |
| CN103704275B (en) * | 2013-12-10 | 2015-01-28 | 淮海工学院 | Separation and purification method and application for algae phenolic acids |
| CN109593140A (en) * | 2018-12-29 | 2019-04-09 | 广州暨南生物医药研究开发基地有限公司 | A kind of crispy gracilaria polysaccharide and its preparation method and application |
| CN109593140B (en) * | 2018-12-29 | 2021-04-16 | 广州暨南生物医药研究开发基地有限公司 | Gracilaria crispatus polysaccharide and preparation method and application thereof |
| CN115746160A (en) * | 2022-11-30 | 2023-03-07 | 南方海洋科学与工程广东省实验室(广州) | Method for reducing viscosity of polysaccharide |
| CN115746160B (en) * | 2022-11-30 | 2024-04-02 | 南方海洋科学与工程广东省实验室(广州) | Method for reducing viscosity of polysaccharide |
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