KR20140039681A - A preparation method of b-chitosan from squid-pen for increasing viscosity and physicochemical binding capacity - Google Patents
A preparation method of b-chitosan from squid-pen for increasing viscosity and physicochemical binding capacity Download PDFInfo
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- KR20140039681A KR20140039681A KR1020120106193A KR20120106193A KR20140039681A KR 20140039681 A KR20140039681 A KR 20140039681A KR 1020120106193 A KR1020120106193 A KR 1020120106193A KR 20120106193 A KR20120106193 A KR 20120106193A KR 20140039681 A KR20140039681 A KR 20140039681A
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- 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
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
The present invention relates to a method for producing beta-chitosan with increased viscosity and physicochemical binding force from squid cartilage. Chitosan manufacturing method that can reduce the effect is excellent.
Description
The present invention relates to a method for producing beta-chitosan having increased viscosity and physicochemical binding force from squid cartilage.
Chitosan has received much attention over the last few decades due to a variety of biological activities, such as antibacterial, anticancer, antioxidant and low cholesterol functions. Chitosan is also reported to have several properties, including water and fat absorption, emulsification, and pigment binding.
Chitosan is currently commercially produced with varying degrees of deacetylation and molecular weight from the shells of crabs and shrimps. Chitosan production from crustacean shells generally consists of four stages: demineralization (DM), deproteinization, decoloration and deacetylation. Among these, demineralization is a process of extraction for 0.5 to 3 hours at room temperature using conventionally diluted HCl, and the intense demineralization treatment causes polymer degradation, resulting in a decrease in molecular weight or viscosity.
Squid cartilage is currently discarded as waste at the squid processing plant, but contains 31-49% chitin by dry weight, so it is expected to be used as a useful resource of chitin and chitosan. Squid cartilage is also extremely low in ash content compared to crab shells, so it is believed that chitosan can be produced without the deashing step.
The physicochemical properties of chitosan vary depending on the method of preparation and, consequently, the function. The exclusion of the deashing step in preparing chitosan from squid cartilage is believed to affect the physicochemical properties of chitosan. However, no direct comparison of the effects of demineralization stage on the physicochemical and functional properties of chitosan derived from squid cartilage has been reported.
Accordingly, an object of the present invention is to provide a method for excluding the deashing step in preparing chitosan from squid cartilage.
The above object of the present invention comprises the steps of preparing beta-chitosan from the squid cartilage without going through the ash ash process; Analyzing the components of the prepared beta-chitosan; This was achieved by investigating the physicochemical binding of beta-chitosan and the DPPH radical scavenging activity.
The present invention provides beta-chitosan with improved viscosity and physico-chemical binding force while reducing chitosan production costs due to the reduction of chemical use, shortening of process time, and massive wastewater discharge due to the elimination of deashing step in chitosan production. Has an excellent effect.
1 is a graph showing the water binding and fat binding of chitosan-WDM and chitosan-DM derived from squid cartilage.
Figure 2 is a graph showing the dye binding force of chitosan-WDM and chitosan-DM derived from squid cartilage.
Figure 3 is a graph showing the DPPH radical scavenging ability of chitosan-WDM and chitosan-DM derived from squid cartilage.
The present invention comprises the steps of deproteinization by pulverizing squid cartilage to treat NaOH; De-ashing the deproteinized cartilage by treating with HCl; In the method for producing beta-chitosan by deacetylation of the chitin produced in the deashing step by treating with NaOH, it relates to a method for producing beta-chitosan characterized in that it does not go through the deashing step.
Hereinafter, the present invention will be described in detail with reference to preferred embodiments and experimental examples.
Test Material Preparation
The squid ( Todarodes pacifica ) cartilage of the disclosure material of the present invention was purchased from Dongwoo Industry Co., Ltd. (Pohang, Korea). The purchased squid cartilage was washed with tap water to remove the water-soluble organic matter and the protein attached, and dried at room temperature. The dried squid cartilage (average length 20.7 cm, width 1.1 cm, thickness 0.63 mm) was ground using a Wiley mill (model 4, Thomas Scientific, Swedesboro, NJ, USA) attached with a 2 mm mesh sieve, followed by a sieve vibrator ( Sieve shaker) was used to separate 20 (0.841 mm) and 40 mesh (0.425 mm) sieves, and then stored in opaque plastic bottles. In the present experiment, only squid cartilage having a particle size of 0.425 to 0.841 mm was used.
Commercially refined soybean oil (Ottogi Co., Gyeonggi-do, South Korea) was used for fat-binding capacity (FBC) experiment, and FD & C Red No.40 (disodium salt) was used for dye-binding capacity (DBC) experiment. of 6-hydroxy-5-[(2-methoxy-5-methyl-4-sulfophenyl) azo] -2-naphthalenesulfonic acid) was used. The 2,2-diphenyl-1-picrylhydrazyl (DPPH) used in the antioxidant activity experiment was Sigma-Aldrich Co. (St. Louis, MO, USA). All analyzes of the invention were performed in three replicates.
Hereinafter, specific examples of the present invention will be described in detail with reference to Examples and Experimental Examples, but the scope of the present invention is not limited only to these examples.
Example 1 Preparation of Chitosan from Squid Cartilage
Squid cartilage ground to a particle size of 0.425-0.841 mm was treated with 3% NaOH (1:10, w / v) at 15 psi / 121 ° C. for 30 minutes to remove proteins (deprotein). The deproteinized cartilage was collected in a 100 mesh sieve, and then sufficiently washed with running water and filtered to remove excess water. The deashing process was done by treating 1N HCl with the deproteinized cartilage at a rate of 1:10 (w / v) for 0 or 30 minutes at room temperature. The residue was dried for 4 hours in a 60 ° C. circulating oven after the washing and filtration process as mentioned above. The deacetylation process was performed by treating the chitin obtained through the deashing process with 35% NaOH at 15 psi / 121 ° C. at a ratio of 1:10 (w / v) for 15 minutes. The resulting chitosan was dried for 4 hours in a 60 ° C. circulating oven after the aforementioned washing process. Hereinafter, in the present specification, in the beta-chitosan production process derived from squid cartilage, the chitosan produced without the demineralization (DM) step is produced as the chitosan-WDM (chitosan-without DM), followed by the demineralization step. Chitosans were named Chitosan-DM, respectively.
Experimental Example 1 Analysis of General Components of Squid Cartilage
Moisture content was analyzed using a halogen moisture analyzer (MB45, Ohaus, Greifensee, Switzerland) and nitrogen was analyzed using an elemental analyzer (EA 1110, CE Instruments, Rodano-Milan, Italy). Crude protein content was calculated by multiplying the nitrogen content by 6.25, and the ash was analyzed according to standard AOAC method 942.05. In addition, fat was Soxhlet extractor (Sox 416, Gerhardt, Germany), chitin was analyzed according to the method of Black and Schwartz.
As a result of the analysis, the chemical composition of the squid cartilage used in the present invention was composed of 74.62% crude protein, 0.80% ash, 0.20% fat and 25.50% chitin. Since squid cartilage contains almost no pigment ( L * = 57.14, α * = 2.97, b * = 10.40), the depigmentation step was not performed in the present experiment.
Experimental Example 2: Color, Deacetylation and Viscosity Analysis
The physicochemical properties of the squid cartilage derived beta-chitosan prepared in Example 1 were examined. That is, the color was measured three times with the color difference meter Minolta Chroma Meter CR-200 (Minolta Camera Co. Ltd, Osaka, Japan) using the light source C, and the results were L * value (lightness) and α * value ( redness, redness,-greenness) and b * values (yellowness, yellowness). Deacetylation degree was measured using N / 400 potassium polyvinyl sulfate (f = 1.00, Wako Pure Chemical Ind., Osaka, Japan) according to the colloid titration method. The viscosity of the chitosan solution was measured using a Brookfield viscometer (model LVDV-II +, Brookfield Engineering Labs., Stoughton, MA, USA) after dissolving chitosan in 0.5% (w / v) concentration in 1% (v / v) acetic acid. It was. Viscosity was measured at 3.96 s −1 shear rate at 25 ± 0.3 ° C. after adding 8 mL of solution to the sample adapter.
Experimental results As shown in Table 1, no significant difference was observed in the water content and the deacetylation degree of chitosan-WDM and chitosan-DM. vs. 0.13%) and viscosity (936.80 mPa s vs. 687.60 mPa s) were observed to be high. The high viscosity (936.80 mPa s) of the chitosan-WDM was determined to result in less depolymerization due to the elimination of the deashing (DM) step.
When measuring color with a color difference meter, chitosan-DM showed somewhat higher L * value, lower α * value, and similar b * value than chitosan-WDM, but both chitosans that were not easily visually observed were observed in light gray. It became.
Therefore, it was observed that the physicochemical properties of squid cartilage derived chitosan, especially viscosity and ash, depend on the deashing (DM) process.
Experimental Example 3: Measurement of Physicochemical Bonding Force
The water-binding capacity (WBC) and fat-binding capacity (FBC) of chitosan were measured by the modified method of Wang and Kinsella. That is, after weighing a 15-mL centrifuge tube containing 0.5 g of chitosan, 10 mL of water or soybean oil was added and mixed for 1 minute by a vortex mixer. The centrifuge tube was left at room temperature for 30 minutes while shaking for 5 seconds at 10 minute intervals, followed by centrifugation at 3,000 rpm for 30 minutes. After removing the supernatant, the centrifuge tube was weighed again to calculate WBC and FBC by Equation 1 below.
In addition, the dye binding strength of chitosan was determined by adding 0.2 g chitosan and 10 mL of water-soluble pigment solution (containing 2.5 mg FD & C Red No. 40) to polypropylene conical tubes using a shaker (100 rpm; MMS-3010, Tokyo Rikakikai Co) according to Cho et al. , Tokyo, Japan) for 1 hour at room temperature. The amount of pigment bound to chitosan was determined by the difference in concentration between the initial dye solution and the filtrate. Dye-binding capacity (DBC) is expressed as% adsorption capacity.
As shown in FIGS. 1 and 2, chitosan-WDM showed a similar pigment binding force (89.9% vs. 89.7%) as compared to chitosan-DM, while water binding force (607.0% vs. 529.9%) and fat binding force. (187.3% vs. 183.5%) showed a high binding force. Therefore, in the present invention, chitosan-WDM having a high viscosity was found to be somewhat superior in water binding and fat binding strength compared to chitosan-DM having a low viscosity.
Experimental Example 4 Investigation of DPPH Radical Scavenging Capacity
The DPPH radical scavenging ability of chitosan was measured by some modification of the Blois method. That is, 0.4 mL of chitosan solution dissolved in 0.5% (w / v) chitosan in 1% (v / v) acetic acid was added to 3 mL of 0.1 mmol DPPH radical ethanol solution and mixed well. Stored. DPPH free radical scavenging ability was calculated by Equation 2 below by measuring the absorbance at 517 nm using a UV / VIS spectrophotometer (Optizen 3220UV, Mecasys Co., Ltd., Korea).
As shown in FIG. 3, chitosan-WDM showed somewhat lower DPPH radical scavenging ability (10.4% vs. 11.4%) than chitosan-DM.
It is known that the DPPH radical scavenging ability of chitosan increases with decreasing molecular weight or viscosity. Therefore, it was confirmed that the chitosan-DM having low viscosity (687.60 mPa s) observed in the present experiment slightly increased DPPH radical scavenging ability compared to the chitosan-WDM having high viscosity (936.80 mPa s).
As described above, the present invention has an excellent effect of providing a chitosan manufacturing method that can reduce the production cost of chitosan by reducing the use of chemicals, shortening the process time and reducing the amount of waste water discharge due to the elimination of the de-ash step. It is a very useful invention in the value added food industry.
Claims (3)
Method for producing beta-chitosan characterized in that it does not go through the deashing step.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104693318A (en) * | 2015-03-24 | 2015-06-10 | 中国科学院海洋研究所 | Beta-chitosan preparation method |
| WO2019064231A1 (en) * | 2017-09-27 | 2019-04-04 | Association For The Advancement Of Tissue Engineering And Cell Based Technologies & Therapies (A4Tec) - Associação | High molecular weight chitosan, process for obtaining and uses thereof |
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- 2012-09-25 KR KR1020120106193A patent/KR20140039681A/en not_active Application Discontinuation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104693318A (en) * | 2015-03-24 | 2015-06-10 | 中国科学院海洋研究所 | Beta-chitosan preparation method |
| WO2019064231A1 (en) * | 2017-09-27 | 2019-04-04 | Association For The Advancement Of Tissue Engineering And Cell Based Technologies & Therapies (A4Tec) - Associação | High molecular weight chitosan, process for obtaining and uses thereof |
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