Method for extracting pectin using enzymes and pectin extracted thereby

Abstract

The present invention relates to a method for extracting pectin from citrus peel with high yield using a combination of an acid, a base, and an enzyme, the method comprising the steps of: a) drying citrus peel; b) pulverizing the dried citrus peel into powder; c) primarily washing the powdered citrus peel; d) primarily centrifuging the washed citrus peel to obtain a first solid; e) adding a solvent to the obtained first solid to obtain an extract; f) secondarily washing the extract; g) secondarily centrifuging the washed extract to obtain a second solid; h) adding an enzyme to the obtained second solid to obtain a reaction mixture; i) thirdly washing the obtained reaction mixture; and j) thirdly centrifuging the washed reaction mixture to obtain pectin.

Description

Pectin extraction method using enzymes to extract pectin and pectin extracted thereby

[0001] The present invention relates to a pectin extraction method for extracting pectin using an enzyme and to pectin extracted thereby.

[0002] Advances in agricultural technology have led to increased fruit production. This has led to increased industrial utilization of fruit, and the increased production of processed products such as fruit juice and fruit wine has led to the generation of byproducts and waste products such as fruit peels and pomace.

[0003] However, these peels contain effective ingredients such as flavonoids and pectin.

[0004] Pectin is a major component of plant cell membranes. It is insoluble in alcohol and acetic acid, and has the ability to form a gel in the presence of an appropriate amount of acid and sugar. It is a polygalacturonic acid in which some of the organic acid groups in the molecule are methyl esters. Therefore, pectin can be said to be a general name for pectinic acid, or neutral salts, acid salts, or mixtures of pectinic acid.

[0005] Pectin is currently used as a gelling agent, stabilizer, and thickener in foods, medicines, and cosmetics. In addition to its function as an additive, its special functions on the human body have been revealed to include lowering blood sugar levels, lowering cholesterol levels, preventing overeating due to a feeling of fullness, removing toxic substances and heavy metals from the body, and strengthening immune function due to its structural and three-dimensional characteristics.

[0006] Accordingly, the inventors of the present invention have completed the present invention by providing a method for extracting pectin from a peel at a high yield using a combination of acid, base, and enzyme.

[0007] The problem to be solved by the present invention is to provide a method for extracting pectin from fruit peel at a high yield by using a combination of acid, base, and enzyme.

[0008] One aspect of the present invention is a pectin complex extraction method comprising the steps of: a) drying citrus peel; b) crushing the dried citrus peel into powder; c) first washing the powdered citrus peel; d) centrifuging the washed citrus peel to obtain a first solid; e) adding a solvent to the obtained first solid to obtain an extract; f) second washing the extract; g) second centrifuging the washed extract to obtain a second solid; h) adding an enzyme to the obtained second solid to obtain a reactant; i) third washing the obtained reactant; and j) third centrifuging the washed reactant to obtain pectin.

[0009] In the present invention, in step a), drying can be performed at 40 to 60°C for 12 to 36 hours.

[0010] In the present invention, in step c), washing may be washing with 70 to 100% (v / v) ethanol.

[0011] In the present invention, in step d), centrifugation may be performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

[0012] In the present invention, in step e), the pH of the solvent may be 2 to 6.

[0013] In the present invention, in step e), the solvent may be a mixed solvent containing oxalic acid and ammonium oxalate.

[0014] In the present invention, in step e), extraction can be performed at 70 to 120°C for 0.5 to 2 hours.

[0015] In the present invention, in step f), washing may be washing with 70 to 100% (v / v) ethanol.

[0016] In the present invention, in step g), centrifugation can be performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

[0017] In the present invention, in step h), the enzyme is pancreatin, and the concentration may be 1 to 8 USP IU / mg.

[0018] In the present invention, in step h), the reaction can be carried out at 100 to 150 rpm for 0.5 to 2 hours.

[0019] In the present invention, in step i), washing may be washing with 70 to 100% (v / v) ethanol.

[0020] In the present invention, in step j), centrifugation can be performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

[0021] Another aspect of the present invention is pectin manufactured by the above manufacturing method.

[0022] The present invention can extract pectin from a peel at a high yield through a specific process.

[0023] In addition, the present invention can maximize the pectin extraction efficiency by controlling the pH of the extraction solvent through acid and base and using a specific enzyme.

[0024] Figure 1 is a flow chart showing the pectin complex extraction method of the present invention.

[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure pertains. In general, the nomenclature used herein and the experimental methods described below are well known and commonly used in the art.

[0026] The term “extract” in this specification refers to a substance obtained by extracting components from a raw material, and can be obtained through an extraction process using an extraction solvent. It can include an extract, a diluted or concentrated extract, a dried product obtained by drying an extract, or a controlled or purified product thereof.

[0027]

[0028] Figure 1 is a flow chart showing the pectin complex extraction method of the present invention.

[0029] Referring to FIG. 1, the pectin complex extraction method of the present invention includes: a) a step of drying citrus peel; b) a step of crushing and powdering the dried citrus peel; c) a step of first washing the powdered citrus peel; d) a step of first centrifuging the washed citrus peel to obtain a first solid; e) a step of adding a solvent to the obtained first solid to obtain an extract; f) a step of second washing the extract; g) a step of second centrifuging the washed extract to obtain a second solid; h) a step of adding an enzyme to the obtained second solid to obtain a reactant; i) a step of third washing the obtained reactant; and j) a step of third centrifuging the washed reactant to obtain pectin.

[0030] In the present invention, step a) is a step of drying citrus peel. The citrus peel may be the peel of the varieties Cheonhyehyang, Hwanggeumhyang, Redhyang, and Onjumilgam, and preferably the peel of Onjumilgam.

[0031] In step a), drying may be performed at 40 to 60°C for 12 to 36 hours, and preferably at 50°C for 24 hours. If the drying is performed at less than 40°C or for less than 12 hours, the moisture content may be too high, making pulverization difficult. If the drying is performed at more than 60°C or for more than 36 hours, excessive drying may occur, reducing the pectin extraction efficiency.

[0032] In the present invention, step b) is a step of crushing dried citrus peel into powder, thereby facilitating washing and extraction. The powdering can be performed using a conventional crusher. It is preferable to use only powder exceeding 30 mesh in size, which has passed through a 30-mesh screen, of the powdered citrus peel.

[0033] In the present invention, step c) is a step of washing the powdered citrus peel, and the washing may be performed at least once, preferably 1 to 5 times, and more preferably 2 to 4 times. In addition, the solvent during washing may be 70 to 100% (v / v) ethanol, and preferably 80 to 90% (v / v) ethanol. In the above range, the extraction efficiency of pectin can be improved. In addition, the content of ethanol added during washing is 60 to 90% by weight based on 100% by weight of the total of the powdered citrus peel and ethanol.

[0034] In the present invention, step d) is a step of obtaining a first solid by first centrifuging the washed citrus peel, and specifically, a step of removing ethanol remaining after washing.

[0035] Centrifugation can be performed at 3,000 to 5,000 rpm for 5 to 20 minutes, preferably at 3,500 to 4,500 rpm for 8 to 12 minutes, and can be performed at room temperature. If the rpm of centrifugation is less than 3,000 rpm or the performance time is less than 5 minutes, ethanol separation is not easy, and if the rpm exceeds 5,000 rpm or the performance time exceeds 20 minutes, the centrifugation efficiency does not increase significantly, so the above range is preferred.

[0036] In the present invention, step e) is a step of obtaining an extract by adding a solvent to the obtained first solid. In step e), the pH of the solvent may be 2 to 6, preferably 3 to 5, and since the extraction efficiency is excellent in the above pH range, the above range is preferred.

[0037] In addition, in step e), the solvent may be a mixed solvent containing oxalic acid and ammonium oxalate. In the extraction, the content of the first solid may be 0.1 to 10 wt% relative to 100 wt% of the first solid and the solvent, and preferably 0.2 to 5 wt%. If the content of the first solid is less than 0.1 wt% or more than 10 wt%, the extraction efficiency may decrease, and therefore the above range is preferred.

[0038] As an extraction method, a solvent extraction method can be used, and furthermore, the desired extract can be subjected to a conventional fractionation process and purified using a conventional purification method.

[0039] The extraction temperature and time may be 70 to 120°C and 0.5 to 2 hours, preferably 80 to 90°C and 0.8 to 1.2 hours, and extraction may be easy within the above range.

[0040] In the present invention, step f) is a step of washing the extract for the second time to remove other components, etc. The washing may be performed one or more times, preferably 1 to 5 times, and more preferably 2 to 4 times. In addition, the solvent during washing may be 70 to 100% (v / v) ethanol, and preferably 80 to 90% (v / v) ethanol. Within the above range, the extraction efficiency of pectin can be improved. In addition, the content of ethanol added during washing is 60 to 90% by weight relative to 100% by weight of the total extract and ethanol.

[0041] In the present invention, step g) is a step of obtaining a second solid by performing a second centrifugation on the washed extract, and specifically, is a step of removing ethanol remaining after washing.

[0042] Centrifugation can be performed at 3,000 to 5,000 rpm for 5 to 20 minutes, preferably at 3,500 to 4,500 rpm for 8 to 12 minutes, and can be performed at room temperature. If the rpm of centrifugation is less than 3,000 rpm or the performance time is less than 5 minutes, ethanol separation is not easy, and if the rpm exceeds 5,000 rpm or the performance time exceeds 20 minutes, the centrifugation efficiency does not increase significantly, so the above range is preferred.

[0043] In the present invention, step h) is a step of adding an enzyme to the obtained second solid to obtain a reactant. In step h), the enzyme is pancreatin, and the concentration may be 1 to 8 USP IU / mg, preferably 2 to 6 USP IU / mg, and since the extraction efficiency is excellent in the above concentration range, the above range is preferred.

[0044] The above enzyme pancreatin is an enzyme that has the activities of α-amylase, lipase and protease, which break down carbohydrates, fats and proteins.

[0045] In addition, in step h), the reaction can be carried out at pH 6 to 8, at 100 to 150 rpm for 0.5 to 2 hours, and preferably at pH 7, at 110 to 130 rpm for 0.8 to 1.2 hours. In the above pH, rpm, and time ranges, the activity of pancreatin is the best, and thus the reaction is the most active.

[0046] In the present invention, step i) is a step of washing the extract for the third time to remove other components, etc. The washing may be performed at least once, preferably 1 to 5 times, and more preferably 2 to 4 times. In addition, the solvent during the washing may be 70 to 100% (v / v) ethanol, and preferably 80 to 90% (v / v) ethanol. Within the above range, the extraction efficiency of pectin can be improved. In addition, the content of ethanol added during the washing is 60 to 90% by weight relative to 100% by weight of the total reactants and ethanol.

[0047] In the present invention, step j) is a step of obtaining pectin by centrifuging the washed reactant a third time, and specifically, is a step of removing ethanol remaining after washing.

[0048] Centrifugation can be performed at 3,000 to 5,000 rpm for 5 to 20 minutes, preferably at 3,500 to 4,500 rpm for 8 to 12 minutes, and can be performed at room temperature. If the rpm of centrifugation is less than 3,000 rpm or the performance time is less than 5 minutes, ethanol separation is not easy, and if the rpm exceeds 5,000 rpm or the performance time exceeds 20 minutes, the centrifugation efficiency does not increase significantly, so the above range is preferred.

[0049] In the present invention, after step j), the obtained third solid can be freeze-dried to obtain pectin, and the freeze-drying can be performed at -100 to -60°C for 60 to 80 hours, and preferably at -90 to -70°C for 70 to 75 hours.

[0050] Another aspect of the present invention is pectin extracted using the above extraction method. The pectin can be used as a substitute for shortening in confectionery and bakery products, and as a raw material for jams, jellies, and fruit spreads.

[0051] Hereinafter, the present disclosure will be described in more detail through examples.

[0052]

[0053] Example 1

[0054] After drying the citrus peel of the Onjumilgam variety at 50℃ for 24 hours, it was crushed using a general crusher and passed through a 30-mesh sieve to obtain powder that passed through the sieve. Thereafter, the produced powdered citrus peel was washed three times using 85% (v / v) ethanol, and the ethanol content was approximately 75% by weight of the total content of the powdered citrus peel and ethanol.

[0055] Afterwards, the washed citrus peel was centrifuged at 4,000 rpm for 10 minutes at room temperature, the supernatant was removed, and a first solid was obtained. A mixed solvent containing oxalic acid and ammonium oxalate was added to the obtained first solid, and extraction was performed at about 85°C for about 1 hour to obtain an extract. The pH of the mixed solvent was about 4.6, and the content of the first solid was about 0.25 wt% based on the total wt%.

[0056] Thereafter, the obtained extract was washed three times with 85% (v / v) ethanol, and the ethanol content was approximately 75 wt% of the total extract and ethanol content. The washed extract was centrifuged at 4,000 rpm for 10 minutes at room temperature, the supernatant was removed, and a second solid was obtained.

[0057] Afterwards, pancreatin was added to the obtained second solid, and the reaction was performed at pH 7, 37°C, and 120 rpm for 1 hour to obtain a reactant, and the concentration of the enzyme at this time was approximately 4 USP IU / mg.

[0058] Thereafter, the obtained reactant was washed three times with 85% (v / v) ethanol, and the ethanol content was approximately 75 wt% of the total reactant and ethanol content. The washed reactant was centrifuged at 4,000 rpm for 10 minutes at room temperature, the supernatant was removed, and pectin was obtained.

[0059] Afterwards, the pectin was freeze-dried at -80°C for 72 hours. Afterwards, dried pectin was produced by hot air drying at approximately 50°C.

[0060]

[0061] Example 2

[0062] In Example 1, pectin was prepared in the same manner as in Example 1, except that the pH of the mixed solvent was adjusted to 2.

[0063]

[0064] Example 3

[0065] In Example 1, pectin was prepared in the same manner as in Example 1, except that the pH of the mixed solvent was adjusted to 6.

[0066]

[0067] Example 4

[0068] In Example 1, pectin was prepared in the same manner as in Example 1, except that the concentration of pancreatin was set to 1 USP IU / mg.

[0069]

[0070] Example 5

[0071] In Example 1, pectin was prepared in the same manner as in Example 1, except that the concentration of pancreatin was set to 8 USP IU / mg.

[0072]

[0073] Comparative Example 1

[0074] In Example 1, pectin was prepared in the same manner as in Example 1, except that 100% (v / v) ethanol was used instead of a mixed solvent.

[0075]

[0076] Comparative Example 2

[0077] In Example 1, pectin was prepared in the same manner as in Example 1, except that distilled water was used instead of a mixed solvent.

[0078]

[0079] Comparative Example 3

[0080] In Example 1, pectin was prepared in the same manner as in Example 1 except that no enzyme was used.

[0081]

[0082] Experimental example

[0083] The yield of pectin according to Examples 1 to 5 and Comparative Examples 1 to 4 was calculated by the following method, and the results are shown in Table 1 below.

[0084] [measurement method]

[0085] Pectin yield (%): Amount obtained after extraction process (g) / dried citrus peel (g) x 100

[0086]

[0087] Yield (%) Example 135 Example 230 Example 328 Example 429 Example 533 Comparative Example 121 Comparative Example 218 Comparative Example 315

[0088] Referring to Table 1 above, it can be confirmed that Example 1, which uses a mixed solvent and an enzyme according to the present invention, shows a higher yield compared to Comparative Examples 1 to 3.

[0089] Additionally, it can be confirmed that Example 1, in which the pH of the mixed solvent is 4.6 and the enzyme concentration is 4, shows a higher yield than Examples 2 to 5.

[0090]

[0091] In this way, the present invention can extract pectin from the peel at a high yield through a specific process, and can maximize the efficiency of pectin extraction by controlling the pH of the extraction solvent through acid and base and using a specific enzyme.

[0092] The present invention provides an extraction method capable of extracting pectin from a peel with a high yield, and thus can be used in various industries.

Claims

1. a) Step of drying citrus peel; b) A step of crushing and powdering dried citrus peel; c) Step of first washing the powdered citrus peel; d) a step of obtaining a first solid by first centrifuging the washed citrus peel; e) a step of adding a solvent to the obtained first solid to obtain an extract; f) Step of washing the extract a second time; g) a step of obtaining a second solid by performing a second centrifugation on the washed extract; h) a step of adding an enzyme to the obtained second solid to obtain a reactant; i) a step of washing the obtained reactant for the third time; and j) A step of obtaining pectin by centrifuging the washed reactant a third time; A pectin complex extraction method comprising:

2. In paragraph 1, A pectin complex extraction method, wherein in step a) drying is performed at 40 to 60°C for 12 to 36 hours.

3. In paragraph 1, In step c), the washing is performed with 70 to 100% (v / v) ethanol, a pectin complex extraction method.

4. In paragraph 1, A pectin complex extraction method, wherein in step d), centrifugation is performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

5. In paragraph 1, In step e), a pectin complex extraction method wherein the pH of the solvent is 2 to 6.

6. In paragraph 1, A pectin complex extraction method, wherein in step e), the solvent is a mixed solvent containing oxalic acid and ammonium oxalate.

7. In paragraph 1, In step e), a pectin complex extraction method is performed at 70 to 120°C for 0.5 to 2 hours.

8. In paragraph 1, In step f), a pectin complex extraction method is performed by washing with 70 to 100% (v / v) ethanol.

9. In paragraph 1, A pectin complex extraction method, wherein in step g), centrifugation is performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

10. In paragraph 1, A pectin complex extraction method, wherein in step h), the enzyme is pancreatin and the concentration is 1 to 8 USP IU / mg.

11. In paragraph 1, A pectin complex extraction method, wherein in step h), the reaction is carried out at 100 to 150 rpm for 0.5 to 2 hours.

12. In paragraph 1, In step i), a pectin complex extraction method is performed by washing with 70 to 100% (v / v) ethanol.

13. In paragraph 1, A pectin complex extraction method, wherein in step j), centrifugation is performed at 3,000 to 5,000 rpm for 5 to 20 minutes.

14. Pectin manufactured by any one of the manufacturing methods of clauses 1 to 13.

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