CN115490782A - Method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid - Google Patents
Method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid Download PDFInfo
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- CN115490782A CN115490782A CN202211248496.5A CN202211248496A CN115490782A CN 115490782 A CN115490782 A CN 115490782A CN 202211248496 A CN202211248496 A CN 202211248496A CN 115490782 A CN115490782 A CN 115490782A
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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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
- C08B37/0048—Processes of extraction from organic materials
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The invention provides a method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid, and belongs to the technical field of waste recycling in tobacco. According to the invention, the mixed acid composed of the organic acid and the inorganic acid is used as the pH value regulating solution, the acidity of the mixed acid is mild, the pectin is prevented from being hydrolyzed due to too strong acidity while the cell wall is damaged, and the pectin yield is improved; the invention adopts ultrasonic-assisted extraction, enhances the cavitation and wall breaking effects of ultrasonic waves, can act on raw materials, enhances the damage of cell walls, and provides assistance for the subsequent extracting solution to better enter the cell walls and dissolve pectin, thereby effectively improving the yield of the pectin.
Description
Technical Field
The invention relates to the technical field of waste recycling in tobacco, in particular to a method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid.
Background
Tobacco is one of main crops, the planting area of the tobacco is large, and tobacco waste is produced every year. Currently, tobacco waste is mainly used as fertilizer, and many valuable substances contained in the tobacco waste are not developed and utilized, so that resource waste is easily caused. Relevant researches show that (tang tian wide, wangxiang, penqiu, liu huayou, tobacco waste utilization research overview [ J ]. Agriculture and technology, 2012,32 (8): 22-28), valuable substances contained in tobacco waste can be extracted by adopting an extraction technology, and can be used for development and application of new products, so that the tobacco waste can be subjected to harmless treatment and even resource treatment.
Pectin is mainly present between the cell wall and the intercellular layer of the plant, is a matrix polysaccharide in the plant cell wall, is formed by combining hydroxyl groups esterified by methyl esters with different degrees on linear polygalacturonic acid and poly-L-rhamnose galacturonic acid, has the maximum relative molecular mass of about 40 ten thousand, and has white, light yellow, light gray or light brown color. At present, a plurality of raw materials are used for extracting pectin, such as pitaya peel, shaddock peel, watermelon peel and the like, while the method for extracting the pectin from tobacco stems is mainly a traditional single acid extraction method, and the yield of the obtained pectin is low.
Disclosure of Invention
The invention aims to provide a method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid, and the method is high in pectin yield.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid, which comprises the following steps:
mixing tobacco stalk powder, mixed acid and water, adjusting the pH value to 0.5-2.5, and performing ultrasonic extraction to obtain an extracting solution; the mixed acid comprises organic acid and inorganic acid;
and (3) sequentially carrying out decoloring, precipitation, separation and drying on the extracting solution to obtain the pectin.
Preferably, the preparation method of the tobacco stem powder comprises the following steps: soaking tobacco stems in boiling water, and sequentially drying and crushing to obtain tobacco stem powder; the soaking time is 1-2 h.
Preferably, the using amount ratio of the tobacco stem powder to the water is 1g (10-50) mL.
Preferably, the organic acid comprises citric acid monohydrate and acetic acid; the inorganic acid comprises concentrated sulfuric acid.
Preferably, the mixed acid comprises water, concentrated sulfuric acid, citric acid monohydrate and acetic acid; the dosage ratio of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid is (300-600) mL, (20-100) mL, (1-6) g, (5-20) mL.
Preferably, the power of ultrasonic extraction is 100-200W, and the time is 30-70 min.
Preferably, the decoloring process comprises the following steps: mixing the extract with active carbon, and decolorizing in water bath.
Preferably, the mass of the activated carbon is 1% of the mass of the extracting solution, and the temperature of the water bath is 60-93 ℃.
Preferably, the reagent used for precipitation is ethanol; the precipitation is carried out under the standing condition, and the precipitation time is 2 hours.
Preferably, the separation mode is suction filtration; the drying mode is vacuum drying.
The invention provides a method for extracting pectin from tobacco stems by utilizing ultrasonic waves and mixed acid, which adopts the mixed acid consisting of organic acid and inorganic acid as pH value regulating solution, so that the extraction process is carried out in a relatively mild acidic state, the acidity of the mixed acid is stable, the cell wall can be damaged, the pectin is prevented from being hydrolyzed due to over-strong acidity, and the pectin yield is improved; the invention adopts ultrasonic-assisted extraction, enhances the cavitation and wall-breaking effects of ultrasonic waves, can act on raw materials, enhances the damage of cell walls, and provides assistance for the subsequent extracting solution to better enter the cell walls and dissolve pectin out, thereby effectively improving the yield of the pectin. The single acid extraction method has insufficient strength for breaking cell walls, slow solvent permeation rate and slow and uneven wall breaking effect when the acid concentration is unstable.
Compared with the traditional single acid extraction method (organic acid or inorganic acid), the extraction method provided by the invention has the advantages that the extraction rate of pectin in tobacco stems is improved, the extraction method is simple and efficient, the cost is low, the time consumption is short, the pectin yield is higher, the quality is better, and the tobacco stem recycling rate of tobacco waste is higher.
Furthermore, the ultrasonic power used by the invention is smaller, the wall breaking effect can be properly achieved, the pectin yield and quality can be prevented from being reduced due to overlarge ultrasonic, the requirement on equipment is lower, the suction filtration and separation times are fewer (only one suction filtration), the pectin yield is prevented from being reduced due to multiple suction filtration, and the problems that the acid liquor used for single acid extraction corrodes the equipment and has overhigh requirement on the material of the equipment are solved.
Drawings
FIG. 1 is a scanning electron micrograph (5 μm) of untreated tobacco stems;
FIG. 2 is a scanning electron micrograph (5 μm) of the stem powder treated with boiling water in example 3;
FIG. 3 is a scanning electron micrograph (5 μm) of tobacco stems obtained in example 3 after ultrasonic treatment;
FIG. 4 is the appearance of the pectin product prepared in example 3;
fig. 5 shows the results of the toxicity test experiment for the pectin product prepared in example 3.
Detailed Description
The invention provides a method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid, which comprises the following steps:
mixing tobacco stalk powder, mixed acid and water, adjusting the pH value to 0.5-2.5, and performing ultrasonic extraction to obtain an extracting solution; the mixed acid comprises organic acid and inorganic acid;
and (3) sequentially carrying out decoloration, precipitation, separation and drying on the extracting solution to obtain the pectin.
In the present invention, unless otherwise specified, all the materials or reagents required are commercially available products well known to those skilled in the art.
The method comprises the steps of mixing tobacco stem powder, mixed acid and water, adjusting the pH value to 0.5-2.5, and carrying out ultrasonic extraction to obtain an extracting solution.
The source of the tobacco stems is not specially limited, and the stems are separated from the fresh tobacco according to the process well known in the field; before the tobacco stems are used, the tobacco stems are preferably washed clean by using clear water.
In the present invention, the method for preparing tobacco stem powder preferably comprises: soaking tobacco stems in boiling water, and sequentially drying and crushing to obtain tobacco stem powder; the soaking time is preferably 1 to 2 hours, and more preferably 2 hours. The drying and pulverizing processes are not particularly limited in the present invention, and the tobacco stem powder having a desired particle size can be obtained according to a process well known in the art. The tobacco stem is soaked in boiling water, and the enzyme of the tobacco stem is deactivated.
In the present invention, the mixed acid includes an organic acid and an inorganic acid; the organic acid preferably comprises citric acid monohydrate and acetic acid; the inorganic acid preferably comprises concentrated sulfuric acid; the mass fraction of the concentrated sulfuric acid is preferably 98%; more preferably, the mixed acid comprises water, concentrated sulfuric acid, citric acid monohydrate, and acetic acid; the dosage ratio of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid is preferably (300-600) mL, (20-100) mL, (1-6) mL, (5-20) mL, and more preferably 319mL.
The existing method adopts single acid to extract pectin, the single acid is organic acid or inorganic acid, the organic acid is generally milder in acidity, and the damage effect on cell walls is slow and incomplete; inorganic acid is generally strong in acidity, especially strong acid easily causes pectin denaturation in the extraction process, and the stability control difficulty of acidity in the whole extraction process is higher, so that the yield and the quality of pectin are influenced. In the mixed acid used in the invention, concentrated sulfuric acid has strong wall-breaking effect, the cell wall tissue can be better destroyed by proper dosage, and the pectin is not hydrolyzed to influence the yield; the acetic acid can weaken the strong acidity of the sulfuric acid and control the acid strength, but the acetic acid is easy to volatilize in the ultrasonic process, and in order to keep the pH value of the whole extraction process basically unchanged, citric acid monohydrate is added as a supplementary acid, and the citric acid monohydrate is not easy to volatilize, and the acidity is weaker than that of the sulfuric acid and the acetic acid, so that the pH value of the mixed acid can be kept stable as much as possible, and large fluctuation is not easy to generate.
In the present invention, the water is preferably ultrapure water; the dosage ratio of the tobacco stalk powder to water is preferably 1g (10-50) mL, and more preferably 1g (10-30) mL; the mixed acid is preferably used in an amount to achieve the desired pH.
In the invention, the process of mixing the tobacco stalk powder, the mixed acid and the water is preferably to mix the tobacco stalk powder and the water, then add the mixed acid and adjust the pH value of the solution to be 0.5-2.5, and more preferably 1.5-2.0.
In the present invention, the power of the ultrasonic extraction is preferably 100 to 200W, more preferably 125 to 150W; the time is preferably 30 to 70min, and more preferably 40 to 50min; the ultrasonic extraction is preferably carried out in an ultrasonic cleaning apparatus.
After the extracting solution is obtained, the extracting solution is sequentially decolored, precipitated, separated and dried to obtain the pectin.
In the present invention, the decoloring process preferably includes: mixing the extracting solution with active carbon, and decoloring under the condition of water bath; the mass of the activated carbon is preferably 1% of the mass of the extracting solution, and the temperature of the water bath is preferably 60-93 ℃; the time for the decolorization is preferably 60min.
After the decoloration is finished, preferably, the obtained product is subjected to suction filtration while the product is hot, and filtrate is collected and precipitated; the suction filtration is preferably carried out by using a vacuum suction filtration pump; the reagent used for precipitation is preferably absolute ethyl alcohol; the volume of the absolute ethyl alcohol is preferably the same as that of the filtrate obtained after decolorization; the precipitation is preferably carried out under a standing condition, and the precipitation time is preferably 2 hours; the invention completely precipitates pectin by precipitation.
After the precipitation is completed, the invention preferably separates the obtained product; the separation is preferably carried out by suction filtration. The invention separates the precipitated pectin by suction filtration.
After the suction filtration is finished, the pectin slurry is preferably dried; the drying mode is preferably vacuum drying; vacuum drying, and pulverizing to obtain pectin. The drying and pulverizing processes are not particularly limited in the present invention, and may be performed according to processes well known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Separating leaves and stems in fresh tobacco, washing the tobacco stems with clear water, soaking the tobacco stems in boiling water for 2 hours, taking out, drying and crushing to obtain tobacco stem powder;
weighing 5g of the tobacco stem powder in a 500mL conical flask, adding ultrapure water according to a material-liquid ratio of 1 (g: mL), placing in the conical flask, adding mixed acid, wherein the mixed acid is a mixture of water, concentrated sulfuric acid (mass fraction is 98%), citric acid monohydrate and acetic acid, the use amounts of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid are 319mL, 3110 mL in sequence, adjusting the pH value of the solution to 2.0, and placing the obtained mixture in an ultrasonic cleaning instrument with ultrasonic power of 150W for treatment for 40min to obtain a brown extracting solution;
adding activated carbon with the mass of 1% of the extract into the extract, placing in a water bath kettle with the water bath temperature of 93 ℃ for decolorization for 60min, then carrying out suction filtration by using a vacuum suction filtration pump while the extract is hot, and collecting filtrate;
adding equal volume of anhydrous ethanol into the filtrate until the pectin concentrate has flocculent precipitate, standing for 2 hr, vacuum filtering to obtain milky pectin slurry, vacuum drying the pectin slurry, and pulverizing to obtain pectin product with mass of 0.79g.
Example 2
Separating leaves and stems in fresh tobacco, washing the tobacco stems with clear water, soaking the tobacco stems in boiling water for 2 hours, taking out, drying and crushing to obtain tobacco stem powder;
weighing 5g of the tobacco stem powder in a 500mL conical flask, adding ultrapure water according to a material-liquid ratio of 1 (g: mL), placing the mixture in the conical flask, adding mixed acid, wherein the mixed acid is a mixture of water, concentrated sulfuric acid (mass fraction is 98%), citric acid monohydrate and acetic acid, the use amounts of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid are 319mL and 310mL in sequence, adjusting the pH value of the solution to 2.0, and placing the obtained mixture in an ultrasonic power 125W ultrasonic cleaning instrument for treatment for 40min to obtain a brown extracting solution;
adding activated carbon with the mass of 1% of the extract into the extract, placing in a water bath kettle with the water bath temperature of 93 ℃ for decolorization for 60min, then carrying out suction filtration by using a vacuum suction filtration pump while the extract is hot, and collecting filtrate;
adding equal volume of anhydrous ethanol into the filtrate until the pectin concentrate has flocculent precipitate, standing for 2 hr, vacuum filtering to obtain milky pectin slurry, vacuum drying the pectin slurry, and pulverizing to obtain pectin product with mass of 0.82g.
Example 3
Separating leaves and stems in fresh tobacco, washing the tobacco stems with clear water, soaking the tobacco stems in boiling water for 2 hours, taking out, drying and crushing to obtain tobacco stem powder;
weighing 5g of the tobacco stem powder in a 500mL conical flask, adding ultrapure water according to a material-liquid ratio of 1 (g: mL), placing in the conical flask, adding mixed acid, wherein the mixed acid is a mixture of water, concentrated sulfuric acid (mass fraction is 98%), citric acid monohydrate and acetic acid, the use amounts of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid are 319mL, 3110 mL in sequence, adjusting the pH value of the solution to 1.5, and placing the obtained mixture in an ultrasonic cleaning instrument with an ultrasonic power of 125W for treatment for 40min to obtain a brown extracting solution;
adding activated carbon with the mass of 1% of the extract into the extract, placing in a water bath kettle with the water bath temperature of 93 ℃ for decolorization for 60min, then carrying out suction filtration by using a vacuum suction filtration pump while the extract is hot, and collecting filtrate;
adding equal volume of anhydrous ethanol into the filtrate until the pectin concentrate appears flocculent precipitate, standing for 2 hr, vacuum filtering to obtain milky pectin slurry, vacuum drying the pectin slurry, and pulverizing to obtain pectin product with a mass of 0.89g.
Comparative example 1
Separating leaves and stems in fresh tobacco, washing the tobacco stems clean with clear water, soaking the tobacco stems in boiling water for 2 hours, taking out the tobacco stems, drying and crushing the tobacco stems to obtain tobacco stem powder;
weighing 5g of tobacco stem powder into a 500mL conical flask, adding ultrapure water according to a material-liquid ratio of 1 (g: mL) to 30, adjusting the pH value to 1.5 by adopting hydrochloric acid with the mass fraction of 38%, and performing ultrasonic extraction for 40min under the condition of the ultrasonic power of 125W to obtain an extracting solution;
adding activated carbon with an amount of 1% of the extract into the extract, heating in a water bath kettle with a water bath temperature of 93 deg.C for 60min, vacuum-filtering with a vacuum pump when the extract is hot, and collecting the filtrate;
adding equal volume of anhydrous ethanol into the filtrate until the pectin concentrate has flocculent precipitate, standing for 2 hr, vacuum filtering to obtain milky pectin slurry, vacuum drying the pectin slurry, and pulverizing to obtain pectin product with pectin weight of 0.49g.
Characterization and Performance testing
1) FIG. 1 is a scanning electron micrograph (5 μm) of untreated tobacco stems; FIG. 2 is a scanning electron micrograph (5 μm) of the stem powder treated with boiling water in example 3; as can be seen from the comparison between FIG. 1 and FIG. 2, the tobacco stems after the enzyme deactivation treatment by boiling water have a larger pulverization degree, which is convenient for the subsequent further extraction.
2) FIG. 3 is a scanning electron micrograph (5 μm) of tobacco stems obtained in example 3 after ultrasonic treatment; as can be seen from fig. 3, after the ultrasonic-assisted solvent extraction, the fibrous tissue part of the tobacco stems is further destroyed, which can promote the dissolution of pectin.
3) FIG. 4 is an appearance diagram of a pectin product prepared in example 3; as shown in figure 4, the appearance color of the extracted pectin is light brown, and the pectin is determined to meet the national standard for the appearance color of the pectin according to the color requirement (GB 25533-2010 national food safety standard pectin).
4) The pectin prepared in example 3 was tested for toxicity and compared to commercially available pectin standards by the following methods: (1) cell recovery: putting 3mL of a mixed solution of a DMEM high-sugar medium and liver cancer cells (random cells in a laboratory) into a centrifuge, centrifuging for 3min at the speed of 1000rpm, taking out, adding 3mL of the medium to prepare a mixed solution, adding the mixed solution and the medium into a culture dish according to the volume ratio of 1 (v/v);
(2) Cell passage: cleaning hepatocarcinoma cell with 2mL PBS, adding pancreatin to separate hepatocarcinoma cell, adding 3mL culture medium, transferring into centrifuge tube, centrifuging for 3min, taking out, adding PBS to clean hepatocarcinoma cell, adding 3mL culture medium, sucking 1mL mixed solution into culture dish, adding 9mL culture medium, adding CO 2 Continuously culturing in an incubator;
(3) Cell receiving plate: adding pancreatin into a culture dish to separate liver cancer cells, adding 3mL of culture medium to wash the liver cancer cells, mixing the washed liver cancer cells with the culture medium, transferring the mixture into a centrifuge tube, centrifuging the centrifuge tube for 3min, taking out the mixture, sucking a small amount of the mixture on a counting plate, measuring the concentration of the liver cancer cells on the counting plate by using Count Star software, calculating the volume of the culture medium and the volume of the liver cancer cells according to the volume of the culture medium and the volume of the liver cancer cells, preparing the liver cancer cell mixed solution with required concentration, transferring the mixed solution into a 96-hole culture plate by using a discharge gun, filling the edge of the mixed solution with PBS buffer solution, and putting CO into the 96-hole culture plate 2 Culturing in an incubator;
(4) Cell loading: weighing pectin sample and commercially available pectin sample 9mg respectively, dissolving with DMSO, adding 864 μ L culture medium to obtain mother liquor containing pectin (1 mg. ML) -1 ) The preparation was carried out according to the set concentration gradient (100. Mu.g/mL, 200. Mu.g/mL, 300. Mu.g/mL, 400. Mu.g/mL and 500. Mu.g/mL). The liquid in the 96-well plate (8 rows × 12 columns) was drained, the outermost periphery was filled with PBS cleaning solution, and the inner region (6 rows × 10 columns) was injected with test samples, wherein the first 5 columns were blank samples without mother liquor, filled with culture medium only, and the last 5 columns were pectin samples or standard solutions with different concentration gradients, and then the 96-well plate was put into a carbon dioxide incubator at the same time. Each sample was set up for 6 sets of parallel experiments;
(5) Adding MTT: weighing the required substancesMTT and PBS buffer were mixed in an amount of 0.5 mg/mL -1 MTT solution, sucking out the liquid in 96-well plate, adding 200. Mu.L MTT solution into 96-well culture plate, and adding CO 2 Taking out the culture box after 4 hours;
(6) Adding DMSO (dimethyl sulfoxide): from CO 2 The plates were removed from the incubator and 200. Mu.L of LDMSO was added to each well, followed by shaking on a shaker for 20min and measuring the absorbance using a microplate reader.
The cell viability calculation formula is as follows:
the results of the toxicity test are shown in Table 1 and FIG. 5.
TABLE 1 pectin toxicity test results
The values of each histogram in FIG. 5 are the average values of the cell viability for each concentration. The cell viability experiment results of table 1 and fig. 5 show that the pectin extracted by the method has slightly less influence on the cell viability than standard pectin, so that the pectin extracted by the method has relatively good quality.
5) And (3) carrying out vacuum filtration on the pectin samples extracted under different conditions by adopting a filtration funnel and qualitative filter paper, then putting the pectin and the filter paper into a vacuum drying oven for drying, and weighing.
The calculation formula of the pectin yield is as follows:
wherein m is 1 : mass of pectin + filter paper, g; m is 2 : mass of filter paper, g; m is a unit of 3 : mass of dried tobacco stalk powder, g. The results are shown in Table 2.
TABLE 2 pectin yields for examples 1-3 and comparative example 1
As can be seen from Table 2, the yield of pectin extracted by the method of the present invention is significantly higher than that of pectin extracted by a single acid in comparative example 1.
6) The pectin prepared in example 3 was subjected to an esterification degree experiment: (1) Weighing 0.2g pectin with an electronic balance, transferring to a conical flask, sequentially adding ethanol and ultrapure water into the conical flask, respectively weighing 2mL and 20mL, stirring with a glass rod until the pectin is dissolved, adding phenolphthalein reagent into the conical flask, and simultaneously using the pectin with a concentration of 0.1 mol.L -1 Was titrated against NaOH solution. When the mixed solution turns red and does not fade for half a minute, the amount of titrated sodium hydroxide is recorded and the volume of titrated sodium hydroxide is recorded as V 1 。
(2) Continuously adding 10mL of 0.1 mol.L concentration into the mixed solution -1 The NaOH solution is placed on a shaking table for shaking for 120min, and then 10mL of NaOH solution with the concentration of 0.1 mol.L is added into the solution -1 HCL solution of (2).
(3) Adding 5 drops of phenolphthalein indicator solution, and adding 0.1 mol.L -1 The NaOH solution was titrated to a pink hue and after no fading within 30s was recorded as the end point of the titration and the volume of NaOH solution consumed was recorded as V 2 。
The pectin esterification degree calculation formula is as follows:
wherein: v 1 Initial titration volume of sample, mL; v 2 Saponification titration volume of sample solution, mL. The results of the two calculations are shown in Table 3.
TABLE 3 pectin esterification degree results
As can be seen from Table 3, the esterification degrees measured by the two experimental results are 76.92% and 73.86%, respectively, and the average value of the two is 75.39%, according to the requirement of industrial production standards on the esterification degree of pectin, the pectin extracted by the method disclosed by the invention reaches the standard of high-ester quick-setting pectin (> 70%), and can be used for preparing fruit juice beverages.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for extracting pectin from tobacco stems by using ultrasonic waves and mixed acid comprises the following steps:
mixing tobacco stem powder, mixed acid and water, adjusting the pH value to 0.5-2.5, and performing ultrasonic extraction to obtain an extracting solution; the mixed acid comprises organic acid and inorganic acid;
and (3) sequentially carrying out decoloration, precipitation, separation and drying on the extracting solution to obtain the pectin.
2. The method according to claim 1, wherein the method for preparing tobacco stem powder comprises: soaking tobacco stems in boiling water, and sequentially drying and crushing to obtain tobacco stem powder; the soaking time is 1-2 h.
3. The method as claimed in claim 2, wherein the ratio of the tobacco stem powder to water is 1g (10-50) mL.
4. The method of claim 1, wherein the organic acid comprises citric acid monohydrate and acetic acid; the inorganic acid comprises concentrated sulfuric acid.
5. The method of claim 1 or 4, wherein the mixed acid comprises water, concentrated sulfuric acid, citric acid monohydrate, and acetic acid; the dosage ratio of the water, the concentrated sulfuric acid, the citric acid monohydrate and the acetic acid is (300-600) mL, (20-100) mL, (1-6) g, (5-20) mL.
6. The method of claim 1, wherein the power of the ultrasonic extraction is 100-200W and the time is 30-70 min.
7. The method of claim 1, wherein the decolorizing comprises: mixing the extract with active carbon, and decolorizing in water bath.
8. The method according to claim 7, wherein the mass of the activated carbon is 1% of the mass of the extracting solution, and the temperature of the water bath is 60-93 ℃.
9. The method according to claim 1, wherein the reagent used for precipitation is ethanol; the precipitation is carried out under the standing condition, and the precipitation time is 2 hours.
10. The method of claim 1, wherein the separation is by suction filtration; the drying mode is vacuum drying.
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| CN102260355A (en) * | 2011-08-26 | 2011-11-30 | 重庆恒远晋通科技有限公司 | Method for extracting pectin based on tobacco |
| CN104710544A (en) * | 2015-03-31 | 2015-06-17 | 川渝中烟工业有限责任公司 | Method for extracting pectin from tobacco waste by using ultrasonic and organic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260355A (en) * | 2011-08-26 | 2011-11-30 | 重庆恒远晋通科技有限公司 | Method for extracting pectin based on tobacco |
| CN104710544A (en) * | 2015-03-31 | 2015-06-17 | 川渝中烟工业有限责任公司 | Method for extracting pectin from tobacco waste by using ultrasonic and organic acid |
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| Title |
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| 肖厚荣等: ""从烟梗中提取果胶工艺研究"" * |
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