CN114989325B - Ultrasonic extraction process for reducing viscosity of tamarind xyloglucan - Google Patents
Ultrasonic extraction process for reducing viscosity of tamarind xyloglucan Download PDFInfo
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- CN114989325B CN114989325B CN202210647229.9A CN202210647229A CN114989325B CN 114989325 B CN114989325 B CN 114989325B CN 202210647229 A CN202210647229 A CN 202210647229A CN 114989325 B CN114989325 B CN 114989325B
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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
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
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Abstract
The invention discloses an ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, which comprises the following steps of: (1) Peeling tamarind seeds, crushing, degreasing and deproteinizing to obtain defatted and deproteinized tamarind kernel powder; (2) Mixing defatted and deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 30-35 mL, carrying out ultrasonic treatment at a temperature of 65-75 ℃ and a W of 170-180 for 85-95 min, standing, centrifuging, mixing the supernatant with an ethanol solution, standing at a temperature of 3-5 ℃ for 1.5-2.5 h, filtering to obtain white precipitate, washing, redissolving in water, and carrying out vacuum freeze drying to obtain the tamarind xyloglucan. The invention adopts the ultrasonic extraction process, has simple and convenient operation, can reduce the molecular weight of the polysaccharide product, further reduce the viscosity of the polysaccharide product, has better physiological activity, can improve the yield of the polysaccharide, and can not influence the primary structure of the polysaccharide.
Description
Technical Field
The invention belongs to the technical field of plant polysaccharide extraction, and particularly relates to an ultrasonic extraction process for reducing viscosity of tamarind xyloglucan.
Background
Tamarind (Tamarindus indica l.) belongs to dicotyledonous plants, the seeds of which are byproducts of the processing of tamarind pulp, consisting of 30% shells and 70% kernels. The tamarind kernel contains more polysaccharide, and the polysaccharide content is 80.66% calculated by using a differential method. Tamarind polysaccharides belong to the xyloglucan family.
Xyloglucan (XyG) is a class of plant cell wall polysaccharides that is found in essentially all plants, differing in content. In dicotyledonous plants, particularly tamarind kernels, the content of XyG is high, so tamarind kernels are one of the most abundant sources of XyG, and many studies thereof have been made.
Tamarind XyG is a polysaccharide substance present in tamarind kernels and can be dissolved in water to form a viscous aqueous solution, and has physiological activities of reducing blood sugar, reducing blood lipid, and improving inflammation. Generally, the yield of XyG (WE-XyG) extracted by water is low, the time consumption is long, and the diffusion capability in biological tissues is weak due to the larger molecular weight; the greater viscosity is detrimental to its uniform mixing with other materials, further, it is hindered from being applied to the fields of foods, medicines and the like. Acid or base extraction of tamarind XyG has been used by existing researchers to increase its yield. However, since the aqueous solution of tamarind kernel powder is viscous, the method of adding acid or alkali is not easy to operate, has large error and low repeatability. For high viscosity XyG, researchers typically use glycosidase treatments to reduce their viscosity for application. But this approach adds cost and operating steps that are not practical. Therefore, it is necessary to find a suitable extraction method to effectively increase the yield of tamarind XyG, and reduce the molecular weight and viscosity thereof to increase the economic benefit thereof.
Disclosure of Invention
Aiming at the prior art, the invention provides an ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan, so as to reduce the problems of high viscosity and high operation difficulty of the xyloglucan in the existing extraction process.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: an ultrasonic extraction process for reducing viscosity of tamarind xyloglucan is provided, comprising the following steps:
(1) Peeling tamarind seeds, crushing, degreasing and deproteinizing to obtain defatted and deproteinized tamarind kernel powder;
(2) Mixing defatted and deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 30-35 mL, carrying out ultrasonic treatment at a temperature of 65-75 ℃ and a W of 170-180 for 85-95 min, standing, centrifuging, mixing the supernatant with an ethanol solution, standing at a temperature of 3-5 ℃ for 1.5-2.5 h, filtering to obtain white precipitate, washing, redissolving in water, and carrying out vacuum freeze drying to obtain the tamarind xyloglucan.
On the basis of the technical scheme, the invention can be improved as follows.
Further, peeling comprises the steps of: washing tamarind seeds, soaking the tamarind seeds in warm water at 80 ℃ for 3-5 hours, drying the tamarind seeds at 70-90 ℃ for 5-7 hours, and removing seed coats.
Further, the crushing comprises the following steps: pulverizing peeled tamarind seed, and sieving with 40 mesh sieve.
Further, degreasing comprises the steps of: mixing the crushed tamarind seeds with n-hexane, degreasing at 65-75 ℃ for 3-5 h, removing the upper layer liquid, and standing at room temperature until the n-hexane is completely volatilized.
Further, deproteinization comprises the steps of: mixing defatted tamarind seeds with water according to the feed liquid ratio of 1 g:9-11 mL, regulating the pH to 9-10 by NaOH, stirring for 25-35 min, centrifuging at 3-5 ℃ for 10-20 min at 4000-6000 r/min, removing supernatant, mixing with water according to the feed liquid ratio of 1 g:9-11 mL, regulating the pH to 6.5-7.0 by using an HCL solution of 0.8-1.2 moL/L, and drying the precipitate.
Further, the centrifugation temperature is 15-25 ℃, the centrifugation speed is 5000-7000 r/min, and the centrifugation time is 15-25 min.
Further, the concentration of the ethanol solution is 94-98 wt%, and the volume ratio of the ethanol solution to the supernatant is 1:2.
Further, the washing is to wash with 94-98 wt% ethanol and absolute ethanol in sequence.
Further, the freezing temperature is-70 to-90 ℃.
The beneficial effects of the invention are as follows:
1. the invention increases the movement frequency and speed of the substance molecules by ultrasonic wave, enhances the penetrating power of the extraction medium, ensures that the extraction medium can be contacted with the target component rapidly and effectively, and accelerates the dissolution of the target component.
2. The invention adopts the ultrasonic extraction process, has simple and convenient operation, can reduce the molecular weight of the polysaccharide product, further reduce the viscosity of the polysaccharide product, has better physiological activity, can improve the yield of the polysaccharide, and can not influence the primary structure of the polysaccharide.
Drawings
FIG. 1 is an FTIR spectrum of ultrasonic extraction of xyloglucan (UAE-XyG) and water extraction of xyloglucan (WE-XyG).
Detailed Description
The following describes the present invention in detail with reference to examples.
Example 1
An ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, comprising the following steps:
(1) Cleaning tamarind seeds, soaking in 80deg.C warm water for 4 hr, oven drying at 80deg.C for 6 hr, removing seed coat, pulverizing peeled tamarind seeds, and sieving with 40 mesh sieve to obtain pulverized tamarind seeds;
(2) Mixing the crushed tamarind seeds with n-hexane, degreasing at 69 ℃ for 4 hours, removing upper liquid, and standing at room temperature until the n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) Mixing defatted tamarind seeds with water according to a feed-liquid ratio of 1g to 10mL, regulating the pH to 9.5 by NaOH, stirring for 30min, centrifuging at 4 ℃ for 15min at 5000r/min, discarding supernatant, mixing with water according to a feed-liquid ratio of 1g to 10mL, regulating the pH to 6.8 by using a HCL solution of 1moL/L, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) Mixing deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 33mL, carrying out ultrasonic treatment at 71 ℃ and 175W for 91min, standing for 24h, centrifuging at 20 ℃ and 6000r/min for 20min, mixing the supernatant with 96wt% ethanol solution according to a volume ratio of 1:2, standing for 2h at 4 ℃, filtering to obtain white precipitate, sequentially washing with 96wt% ethanol and absolute ethanol, redissolving in water, and carrying out vacuum freeze drying at-808 ℃ to obtain tamarind xyloglucan.
Example 2
An ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, comprising the following steps:
(1) Cleaning tamarind seeds, soaking in 80deg.C warm water for 3 hr, oven drying at 70deg.C for 7 hr, removing seed coat, pulverizing peeled tamarind seeds, and sieving with 40 mesh sieve to obtain pulverized tamarind seeds;
(2) Mixing the crushed tamarind seeds with n-hexane, degreasing at 65 ℃ for 5 hours, removing upper liquid, and standing at room temperature until the n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) Mixing defatted tamarind seeds with water according to a feed-liquid ratio of 1g to 9mL, regulating the pH to 9 with NaOH, stirring for 25min, centrifuging at 3 ℃ and 4000r/min for 20min, discarding supernatant, mixing with water according to a feed-liquid ratio of 1g to 9mL, regulating the pH to 6.5 with a HCL solution of 0.8moL/L, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) Mixing deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 30mL, carrying out ultrasonic treatment at 65 ℃ and 170W for 95min, standing for 24h, centrifuging at 15 ℃ and 5000r/min for 25min, mixing the supernatant with 94wt% ethanol solution according to a volume ratio of 1:2, standing at 3 ℃ for 1.5h, filtering to obtain white precipitate, washing 94wt% ethanol and absolute ethanol in sequence, redissolving in water, and carrying out vacuum freeze drying at-70 ℃ to obtain tamarind xyloglucan.
Example 3
An ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, comprising the following steps:
(1) Cleaning tamarind seeds, soaking in 80 ℃ warm water for 5 hours, drying at 90 ℃ for 5 hours, removing seed coats, crushing peeled tamarind seeds, and sieving with a 40-mesh sieve to obtain crushed tamarind seeds;
(2) Mixing the crushed tamarind seeds with n-hexane, degreasing at 75 ℃ for 3 hours, removing upper liquid, and standing at room temperature until the n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) Mixing defatted tamarind seeds with water according to a feed-liquid ratio of 1g to 11mL, regulating pH to 10 with NaOH, stirring for 35min, centrifuging at 5 ℃ for 10min at 6000r/min, discarding supernatant, mixing with water according to a feed-liquid ratio of 1g to 11mL, regulating pH to 7.0 with 1.2moL/L HCL solution, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) Mixing deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 35mL, carrying out ultrasonic treatment at 75 ℃ and 180W for 85min, standing for 24h, centrifuging at 25 ℃ and 7000r/min for 15min, mixing the supernatant with 98wt% ethanol solution according to a volume ratio of 1:2, standing for 2.5h at 5 ℃, filtering to obtain white precipitate, washing 98wt% ethanol and absolute ethanol in sequence, redissolving in water, and carrying out vacuum freeze drying at-90 ℃ to obtain tamarind xyloglucan.
Comparative example 1
The ultrasonic power in step (4) in example 1 was changed to 200W.
Comparative example 2
The ultrasonic temperature in step (4) in example 1 was changed to 60 ℃.
Comparative example 3
The ultrasonic time in step (4) in example 1 was changed to 100 minutes.
Comparative example 4
The ratio of the tamarind kernel powder to water in step (4) of example 1 was changed to 1g:40mL.
Comparative example 5
The ultrasonic treatment in step (4) in example 1 was changed to water bath treatment (WE-XyG).
The yields and viscosities of tamarind xyloglucan in examples and comparative examples were measured as shown in table 1.
TABLE 1 yield and viscosity of tamarind xyloglucan
Fourier infrared spectroscopy (FTIR) analysis was performed on tamarind xyloglucan of the present invention as follows:
accurately weighing 120mg KBr crystal, grinding in a small mortar until fine powder is formed, and tabletting. The sample-free KBr pellet was used and an infrared spectrum scan was performed on an infrared spectrophotometer to collect a reference background spectrum. Mixing 120mg KBr crystal and 2mg tamarind XyG sample, grinding, tabletting, and infrared spectrum scanning (500-4000 cm) -1 )。
FTIR can determine which functional groups or chemical bonds are present or altered in the sample. FIG. 1 is an infrared absorption spectrum of ultrasonic-extracted xyloglucan (UAE-XyG) and water-extracted xyloglucan (WE-XyG). Ultrasonic extraction of xyloglucanThe main peaks of the infrared spectra of the glycans (UAE-XyG) and the water-extracted xyloglucan (WE-XyG) are substantially identical. UAE-XyG and WE-XyG samples at 3418.73cm -1 A broadband appears at this point due to the O-H stretching vibration of the dextran scaffold. The sugar chain skeleton of XyG has three characteristic absorption peaks: CH (CH) 2 Bending, C-O bond extension, and C-C bond vibration. Due to CH 2 Bending at 1375.99cm -1 A sharp frontal surface at 1315.40cm -1 A soft peak is arranged at the position; due to the extension of the C-O bond of the XyG ring, at 1040.83cm -1 A strong peak was observed there; at 1416.29cm -1 The peak appearing at this point is caused by the C-C bond vibration. The result shows that the polysaccharide extracted from tamarind kernel is XyG, and the extraction method adopted by the invention has little influence on the functional group or chemical bond of XyG.
The molecular weight distribution of tamarind xyloglucan according to the present invention was measured as follows, and the results are shown in Table 2.
Table 2 monosaccharide composition and molecular weight of XyG
| Sample of | Ultrasonic extraction of xyloglucan (UAE-XyG) |
| Arabinose (Ara) | 0.174 |
| Glucose (Glu) | 7.832 |
| Galactose (Gal) | 2.029 |
| Xylose (Xyl) | 3.573 |
| Galacturonic acid | 0.045 |
| Glucuronic acid | 0.041 |
| Glu:Xyl:Gal | 3.86:1.76:1 |
| Mw(g/mol) | 1.64×106 |
| PDI(Mw/Mn) | 1.10 |
During the application of tamarind xyloglucan, its properties are often affected by other substances. Salts and sucrose are two substances that are often ingested by the human body and may have an effect on the apparent viscosity of XyG, which in turn affects XyG applications. Apparent viscosities of XyG obtained by the two extraction methods were measured with respect to NaCl solution and sucrose solution having different concentrations, and the results are shown in tables 3 and 4.
TABLE 3 n and K of XyGs solutions at different NaCl concentrations
TABLE 4 n and K of XyGs solutions at different sucrose concentrations
As can be seen from tables 3 and 4, the apparent viscosity of UAE-XyG was always lower than that of WE-XyG at the same NaCl concentration and sucrose concentration.
While specific embodiments of the invention have been described in detail in connection with the examples, it should not be construed as limiting the scope of protection of the patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (6)
1. An ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, which is characterized by comprising the following steps of:
(1) Peeling tamarind seeds, crushing, degreasing and deproteinizing to obtain defatted and deproteinized tamarind kernel powder; the peeling comprises the following steps: washing tamarind seeds, soaking the tamarind seeds in warm water at 80 ℃ for 3-5 hours, drying the tamarind seeds at 70-90 ℃ for 5-7 hours, and removing seed coats; the degreasing comprises the following steps: mixing the crushed tamarind seeds with n-hexane, degreasing at 65-75 ℃ for 3-5 h, removing upper liquid, and standing at room temperature until the n-hexane is completely volatilized; the deproteinization comprises the following steps: mixing defatted tamarind seeds with water according to the feed liquid ratio of 1g to 9-11 mL, regulating the pH to 9-10 by NaOH, stirring for 25-35 min, centrifuging at 3-5 ℃ for 10-20 min at 4000-6000 r/min, removing supernatant, mixing with water according to the feed liquid ratio of 1g to 9-11 mL, regulating the pH to 6.5-7.0 by using an HCL solution with the concentration of 0.8-1.2 moL/L, and drying the precipitate;
(2) Mixing defatted and deproteinized tamarind kernel powder with water according to a feed liquid ratio of 1g to 30-35 mL, carrying out ultrasonic treatment at a temperature of 65-75 ℃ and a W of 170-180 for 85-95 min, standing, centrifuging, mixing the supernatant with an ethanol solution, standing at a temperature of 3-5 ℃ for 1.5-2.5 h, filtering to obtain white precipitate, washing, redissolving in water, and carrying out vacuum freeze drying to obtain the tamarind xyloglucan.
2. The extraction process according to claim 1, wherein the comminution comprises the steps of: pulverizing peeled tamarind seed, and sieving with 40 mesh sieve.
3. The extraction process according to claim 1, characterized in that: the centrifugal temperature is 15-25 ℃, the centrifugal speed is 5000-7000 r/min, and the centrifugal time is 15-25 min.
4. The extraction process according to claim 1, characterized in that: the concentration of the ethanol solution is 94-98 wt%, and the volume ratio of the ethanol solution to the supernatant is 1:2.
5. The extraction process according to claim 1, characterized in that: the washing is to wash with 94-98 wt% ethanol and absolute ethanol in turn.
6. The extraction process according to claim 1, characterized in that: the freezing temperature is-70 to-90 ℃.
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| JP2012012328A (en) * | 2010-06-30 | 2012-01-19 | Dsp Gokyo Food & Chemical Co Ltd | Xyloglucan-cation complex and stabilized composition containing the same |
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| CN114181329A (en) * | 2021-12-27 | 2022-03-15 | 青岛琛蓝海洋生物工程有限公司 | Method for extracting xyloglucan in tamarind seeds |
| CN114507295A (en) * | 2021-12-22 | 2022-05-17 | 云南猫哆哩集团食品有限责任公司 | Preparation method of tamarind seed polysaccharide glue solution |
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| CA2852026C (en) * | 2011-10-12 | 2018-09-18 | Ocean Spray Cranberries, Inc. | Xyloglucan extraction process |
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| JP2012012328A (en) * | 2010-06-30 | 2012-01-19 | Dsp Gokyo Food & Chemical Co Ltd | Xyloglucan-cation complex and stabilized composition containing the same |
| CN108586633A (en) * | 2018-02-08 | 2018-09-28 | 绿麒（厦门）海洋生物科技有限公司 | A kind of quickly water suction is high to be swollen tamarind gum and preparation method thereof |
| CN114507295A (en) * | 2021-12-22 | 2022-05-17 | 云南猫哆哩集团食品有限责任公司 | Preparation method of tamarind seed polysaccharide glue solution |
| CN114181329A (en) * | 2021-12-27 | 2022-03-15 | 青岛琛蓝海洋生物工程有限公司 | Method for extracting xyloglucan in tamarind seeds |
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| High pressure processing of tamarind (Tamarindus indica) seed for xyloglucan extraction;Nipat Limsangouan等;《Food science & technology》;20200909;第134卷;正文全文 * |
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