CN113321751A - Method for extracting red-heart pitaya peel polysaccharide - Google Patents
Method for extracting red-heart pitaya peel polysaccharide Download PDFInfo
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- CN113321751A CN113321751A CN202110807199.9A CN202110807199A CN113321751A CN 113321751 A CN113321751 A CN 113321751A CN 202110807199 A CN202110807199 A CN 202110807199A CN 113321751 A CN113321751 A CN 113321751A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 64
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 64
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 64
- 240000008086 Echinocereus enneacanthus Species 0.000 title claims abstract description 50
- 235000010837 Echinocereus enneacanthus subsp brevispinus Nutrition 0.000 title claims abstract description 50
- 235000006850 Echinocereus enneacanthus var dubius Nutrition 0.000 title claims abstract description 50
- 235000001808 Ceanothus spinosus Nutrition 0.000 title claims abstract description 18
- 241001264786 Ceanothus spinosus Species 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 230000003247 decreasing effect Effects 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000219357 Cactaceae Species 0.000 description 1
- 240000000399 Delphinium grandiflorum Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000007365 immunoregulation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
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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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for extracting red-heart pitaya peel polysaccharide, which comprises the following steps: weighing red-heart pitaya peel powder, placing the red-heart pitaya peel powder into a centrifugal tube, adding distilled water according to a certain material-liquid ratio, and uniformly mixing; placing the cell in an ultrasonic cell crusher, carrying out ice bath, adjusting parameters, and crushing; centrifuging the crushed sample at the rotating speed of 6000r/min to obtain supernatant; putting the supernatant and the AB-8 macroporous adsorption resin into a conical flask according to the mass ratio of 1: 2; placing in a shaking table at 38 deg.C and 150r/min for 2h, vacuum filtering to obtain pitaya peel polysaccharide solution; adding 3 times of absolute ethyl alcohol into the supernatant, precipitating with ethanol at 4 ℃ for 12h, filtering, separating polysaccharide, drying, and weighing the mass of the pure pitaya peel polysaccharide.
Description
Technical Field
The invention relates to the technical field of extraction, in particular to a method for extracting red-heart pitaya peel polysaccharide.
Background
Pitaya (pitaya), native to the tropical desert region of Central America, is a perennial sprawl plant of the family Cactaceae, genus trigonostema. The pitaya peel has extremely high utilization value, and contains a large amount of nutrient substances such as polysaccharide, natural pigment, flavone and the like. Researches show that the plant polysaccharide has multiple effects of immunoregulation, oxidation resistance, antibiosis, disinfection and the like, so that a method for extracting the pericarp polysaccharide of the red-heart pitaya needs to be researched.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for extracting red-heart pitaya peel polysaccharide.
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for extracting red-heart pitaya peel polysaccharide comprises the following steps:
weighing red-heart pitaya peel powder, placing the red-heart pitaya peel powder into a centrifugal tube, adding distilled water according to a certain material-liquid ratio, and uniformly mixing; placing the cell in an ultrasonic cell crusher, carrying out ice bath, adjusting parameters, and crushing; centrifuging the crushed sample at the rotating speed of 6000r/min to obtain supernatant; putting the supernatant and the AB-8 macroporous adsorption resin into a conical flask according to the mass ratio of 1: 2; placing in a shaking table at 38 deg.C and 150r/min for 2h, vacuum filtering to obtain pitaya peel polysaccharide solution; adding 3 times of anhydrous ethanol into the supernatant, precipitating with ethanol at 4 deg.C for 12h, vacuum filtering, separating polysaccharide, drying, weighing the mass of pure pitaya peel polysaccharide, and calculating the extraction rate of pitaya peel polysaccharide according to the following formula:
in the formula: m1 mass of Pitaya pericarp polysaccharide g
m0 mass of pitaya peel powder, g.
As a further improvement of the invention, the pretreatment of the AB-8 macroporous adsorption resin comprises the following steps: weighing a certain amount of AB-8 macroporous adsorption resin, soaking the AB-8 macroporous adsorption resin in deionized water until the AB-8 macroporous adsorption resin swells, and removing the macroporous adsorption resin floating on the surface of water; soaking the sieved macroporous resin in absolute ethyl alcohol for 24 hours, washing with absolute ethyl alcohol until no white turbidity appears, and then washing with deionized water until no ethanol smell appears; adding 3 percent of the mixture, soaking for 3 hours, and washing with deionized water to be neutral; soaking in 3% NaOH solution for 3 hr, and washing with deionized water to neutrality.
As a further improvement of the invention, the parameters of the ultrasonic cell disruptor are set as follows: the ultrasonic time is 25min, the ultrasonic power is 80w, and the material-liquid ratio is 1: 12.
The invention has the advantages of
Compared with the prior art, the invention has the advantages that:
the method can efficiently extract the plant polysaccharide, and has the technical effects of mild conditions, short extraction time and high extraction rate.
Drawings
FIG. 1 is a graph showing the effect of ultrasonic power on polysaccharide extraction rate in accordance with the present invention.
FIG. 2 is a graph showing the effect of sonication time on polysaccharide extraction rate according to the present invention.
FIG. 3 is a graph showing the effect of feed liquid ratio on polysaccharide extraction rate in accordance with the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
1.1 treatment of materials
Drying the pitaya peel in a constant-temperature drying oven at 60 ℃ until the weight is constant, crushing the pitaya peel into powder, and sieving the powder with a 60-mesh sieve for later use.
1.2 pretreatment of AB-8 macroporous adsorbent resin
Weighing a certain amount of AB-8 macroporous adsorption resin, soaking the AB-8 macroporous adsorption resin in deionized water until the AB-8 macroporous adsorption resin swells, and removing the macroporous adsorption resin floating on the surface of water; soaking the sieved macroporous resin in absolute ethyl alcohol for 24 hours, washing with absolute ethyl alcohol until no white turbidity appears, and then washing with deionized water until no ethanol smell appears; adding 3 percent of the mixture, soaking for 3 hours, and washing with deionized water to be neutral; soaking the mixture in 3% NaOH solution for 3 hr, and washing with deionized water to neutrality for use.
1.3 extraction of Pitaya pericarp polysaccharide
Accurately weighing 1g of red-core pitaya peel powder, placing the red-core pitaya peel powder into a 50ml centrifugal tube, adding distilled water according to a certain material-liquid ratio, and uniformly mixing; placing the cell in an ultrasonic cell crusher, carrying out ice bath, adjusting parameters, and crushing; centrifuging the crushed sample for 15min at the rotating speed of 6000r/min to obtain supernatant; putting the supernatant and the AB-8 macroporous adsorption resin into a conical flask according to the mass ratio of 1: 2; placing in a shaking table at 38 deg.C and 150r/min for 2h, vacuum filtering to obtain pitaya peel polysaccharide solution; and adding 3 times of volume of absolute ethyl alcohol into the supernatant, precipitating with ethanol at 4 ℃ for 12h, filtering, separating polysaccharide, drying, and weighing the mass of the pure pitaya peel polysaccharide. The extraction rate of the pitaya peel polysaccharide is calculated according to the following formula.
In the formula: m1 mass of Pitaya pericarp polysaccharide g
m0 mass of pitaya peel powder, g.
1.4 Pitaya pericarp polysaccharide extraction process optimization
1.4.1 Single factor experiment
A single-factor experiment is adopted to explore the influence of ultrasonic power, ultrasonic time and feed liquid ratio on the extraction rate of pitaya peel polysaccharide. The ultrasonic treatment time is 25min, and the material-liquid ratio is 1:8, respectively measuring the extraction effects of ultrasonic powers of 40W, 60W, 80W, 100W and 120W under the low-temperature condition, and screening out the optimal ultrasonic time; and then, using 80w of the highest extraction rate of the pitaya peel polysaccharide as ultrasonic power, setting ultrasonic time to be 10min, 15min, 20min, 25min and 30min, wherein the material-liquid ratio is 1:8, extracting under a low-temperature condition, and optimizing ultrasonic time; based on the above optimal ultrasonic parameters, under the low temperature conditions of ultrasonic time of 25min and ultrasonic power of 80w, the extraction effects of the material-liquid ratios of 1:8, 1:10, 1:12 and 1:16 are respectively determined.
Time, feed-liquid ratio, power parameters
1.4.2 orthogonal experiments
On the basis of results obtained by a single-factor experiment of an ultrasonic-assisted method, three-level orthogonal collocation is further explored on three factors of ultrasonic power, ultrasonic time and a feed-liquid ratio by taking the extraction rate of polysaccharide as an evaluation index.
2.1 Single factor test results
2.1.1 Effect of ultrasonic Power on polysaccharide extraction
The influence of the ultrasonic power on the polysaccharide extraction rate is shown in fig. 1, and the polysaccharide extraction rate can be obtained from fig. 1 and shows a trend that the polysaccharide extraction rate is increased and then decreased with the increase of the ultrasonic power; when the ultrasonic power reaches 80W, the extraction rate of the polysaccharide reaches the highest, and the optimal ultrasonic power for extracting the polysaccharide is determined to be 80W.
2.1.2 Effect of ultrasound time on polysaccharide extraction
The influence of the ultrasonic time on the polysaccharide extraction rate is shown in fig. 2, and the polysaccharide extraction rate shows a trend of firstly decreasing, then increasing and then decreasing with the increase of the ultrasonic time from fig. 2. And when the ultrasonic time is 25min and the extraction rate of the polysaccharide is highest, determining that the optimal ultrasonic time for extracting the polysaccharide is 25 min.
2.1.3 Effect of feed liquid ratio on polysaccharide extraction
The influence of the feed-liquid ratio on the polysaccharide extraction rate is shown in fig. 3, and it can be seen from fig. 3 that the polysaccharide extraction rate is increased and then decreased as the feed-liquid ratio is increased. When the feed-liquid ratio is 1:12, the extraction rate of the polysaccharide is highest, and the optimal feed-liquid ratio for extracting the polysaccharide is determined to be 1: 12.
2.2 results of orthogonal experiments
TABLE 1 results of orthogonal experiments
Table1 Results of orthogonal test
The orthogonal experiment result is shown in table 1, and can be obtained from table 1, the orthogonal experiment result is that the polysaccharide extraction rate of No. 5 tube is maximum and reaches 4.93%, and the corresponding parameters are ultrasonic power of 80W, ultrasonic time of 25min and material-liquid ratio of 1: 12. Through the range comparison of all factors, the influence of the ultrasonic power on the polysaccharide extraction rate is the largest, and the influence degree of the ultrasonic time and the feed-liquid ratio is relatively small and is equivalent.
2.3 conclusion
The research optimizes the extraction process of the red-heart pitaya peel polysaccharide by an ultrasonic auxiliary method and a macroporous resin adsorption method, and the optimal extraction process of the red-heart pitaya peel polysaccharide is determined by a single-factor experiment and an orthogonal experiment as follows: the ultrasonic power is 80w, the ultrasonic time is 25min, the material-liquid ratio is 1:12g/mL, and the extraction rate is 4.90 percent calculated by the ratio of the dried polysaccharide mass to the pitaya peel powder. However, in the research of Delphinium grandiflorum et al on extraction of pitaya peel polysaccharide, absorbance of a glucose standard solution at 490nm is used as a standard curve, the content of polysaccharide in the pitaya peel polysaccharide solution is determined in the standard curve by measuring the absorbance, and the extraction rate of the pitaya peel polysaccharide is calculated to be 13.88%.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (3)
1. A method for extracting red-heart pitaya peel polysaccharide is characterized by comprising the following steps:
weighing red-heart pitaya peel powder, placing the red-heart pitaya peel powder into a centrifugal tube, adding distilled water according to a certain material-liquid ratio, and uniformly mixing; placing the cell in an ultrasonic cell crusher, carrying out ice bath, adjusting parameters, and crushing; centrifuging the crushed sample at the rotating speed of 6000r/min to obtain supernatant; putting the supernatant and the AB-8 macroporous adsorption resin into a conical flask according to the mass ratio of 1: 2; placing in a shaking table at 38 deg.C and 150r/min for 2h, vacuum filtering to obtain pitaya peel polysaccharide solution; adding 3 times of anhydrous ethanol into the supernatant, precipitating with ethanol at 4 deg.C for 12h, vacuum filtering, separating polysaccharide, drying, weighing the mass of pure pitaya peel polysaccharide, and calculating the extraction rate of pitaya peel polysaccharide according to the following formula:
in the formula: m1 mass of Pitaya pericarp polysaccharide g
m0 mass of pitaya peel powder, g.
2. The method for extracting the pericarp polysaccharide of the red-heart pitaya according to claim 1, which is characterized in that:
the pretreatment of the AB-8 macroporous adsorption resin comprises the following steps: weighing a certain amount of AB-8 macroporous adsorption resin, soaking the AB-8 macroporous adsorption resin in deionized water until the AB-8 macroporous adsorption resin swells, and removing the macroporous adsorption resin floating on the surface of water; soaking the sieved macroporous resin in absolute ethyl alcohol for 24 hours, washing with absolute ethyl alcohol until no white turbidity appears, and then washing with deionized water until no ethanol smell appears; adding 3 percent of the mixture, soaking for 3 hours, and washing with deionized water to be neutral; soaking in 3% NaOH solution for 3 hr, and washing with deionized water to neutrality.
3. The method for extracting the pericarp polysaccharide of the red-heart pitaya according to claim 1, which is characterized in that:
the parameters of the ultrasonic cell disruptor are set as follows: the ultrasonic time is 25min, the ultrasonic power is 80w, and the material-liquid ratio is 1: 12.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478817A (en) * | 2022-02-24 | 2022-05-13 | 华南理工大学 | Pitaya peel polysaccharide and preparation method and application thereof |
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|---|---|---|---|---|
| CN109160955A (en) * | 2018-11-05 | 2019-01-08 | 贺州学院 | The method of dragon fruit pericarp extraction polysaccharide |
| CN112029009A (en) * | 2020-09-30 | 2020-12-04 | 海南北纬十八度食品加工有限公司 | Preparation method of pitaya flower polysaccharide |
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- 2021-07-16 CN CN202110807199.9A patent/CN113321751A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160955A (en) * | 2018-11-05 | 2019-01-08 | 贺州学院 | The method of dragon fruit pericarp extraction polysaccharide |
| CN112029009A (en) * | 2020-09-30 | 2020-12-04 | 海南北纬十八度食品加工有限公司 | Preparation method of pitaya flower polysaccharide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114478817A (en) * | 2022-02-24 | 2022-05-13 | 华南理工大学 | Pitaya peel polysaccharide and preparation method and application thereof |
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