Method for producing V-type crystalline starch and use of V-type crystalline starch as seasoning
Patent Information
- Application Number
- JP2023547373
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2022-09-30
- Filing Date
- 2022-11-16
- Publication Date
- 2025-03-07
- Estimated Expiration
- 2042-11-16
AI Technical Summary
【0032】 (1)本発明では、乾熱非晶質化によって澱粉を十分にデクラスタリングし、澱粉の糊化度を90%以上にし、澱粉の濃度を効果的に向上させ、分級澱粉の製造効率を顕著に高める。 (2)本発明では、アルコール沈殿·分級処理により、重合度範囲の異なる分級澱粉を取得し、単一螺旋キャビティのサイズの異なるV型結晶を形成するのに適した澱粉原料が得られる。 (3)本発明では、プラズマ活性水を利用して酸性溶媒環境を提供することによって、澱粉鎖の流動性を高め、澱粉の溶解度を向上させ、より多くの単一螺旋キャビティにより対象分子を捕捉するための部位をより多く提供し、また、周波数可変超音波支援複合化方法と組み合わせることで、風味分子に対して高包埋率や徐放効果があるV6I-、V6II-、V6III-、V7-、及びV8-型結晶澱粉を得ることができる。プラズマ活性水と周波数可変超音波とを組み合わせて複合化したV型結晶澱粉は、短距離秩序や結晶化度が顕著に改善され、このような秩序結晶構造は、包埋される風味分子を安定化させ、環境の変化に対する抵抗性を高めることに有利である。 (4)本発明では、高速冷却及び結晶化方法により結晶核が大量で形成され、適切な温度で保温することにより結晶の成長が促進され、これは、風味分子を複合化したV型結晶澱粉の更なる結晶化や微結晶の更なる大型化に有利であり、結晶構造が完備される傾向があり、これにより、複合物中の風味分子の放出時間を延ばし、複合物の安定性を向上させるのに有利である。 (5)本発明では、風味分子を複合化したV型結晶澱粉中の風味分子の包埋や徐放効果についてさらに試験した。試験の結果、通常の水熱処理を受けた澱粉乳で風味分子を吸着して包埋する場合、吸着率は最高で8.2%である一方、本発明で製造された、風味分子を複合化したV型結晶澱粉では、風味分子の包埋率が最高で68.2%に達する。各種のV型結晶澱粉と複合化した風味分子は、包埋率や徐放効果のいずれも顕著に向上し、V型結晶のいずれの種類も、各種の風味分子の包埋や制御放出に適している。 (6)本発明は、様々な風味分子を用いて、様々な結晶澱粉を形成し、次に、結晶特性を制御することによって貯蔵や後加工中の風味徐放を実現するものであり、得られた風味分子を複合化したV型結晶澱粉では、風味分子の包埋率や徐放効果が従来技術よりも顕著に向上し、澱粉系食品の風味を保持するための新しい技術を提供することが可能となり、従来の風味分子の包埋および徐放技術の発展形であり、そのV型結晶澱粉は、配合材料として澱粉系食品に添加されて食品の風味をよくすることもでき、産業上の付加価値が期待できる。
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Abstract
Description
[Technical field]
[0001] The present invention relates to a method for producing V-type crystalline starch and the use of V-type crystalline starch as a seasoning, and belongs to the fields of food and chemical industries. [Background technology]
[0002] Flavor is an important quality for evaluating the quality of food and is one of the important factors that affect consumer acceptance. In the modern food industry, the retention and controlled release of flavor molecules have been widely paid attention to and researched. As starch-based foods have become commonly eaten, are practical, and are inexpensive, there has been great interest in the complexation of starch with flavor molecules in recent years. As the research progresses, the complexation technology of starch with flavor molecules has matured, and it has been reported that the embedding rate of starch in flavor molecules reaches about 38%, and there is a sustained release effect within 96h (hours). However, the complexation and sustained release effect of starch with flavor molecules need to be further improved.
[0003] At present, research into improving the flavor quality of starch-based foods mainly focuses on the selection of raw materials and technological optimization, such as the selection of superior raw materials, appropriate temperature storage, pre-addition of antioxidants, the use of high-density packaging materials, and the addition of exogenous flavor molecules. However, these methods have little effect and are essentially unable to improve the quality of the products. Summary of the Invention [Problem to be solved by the invention]
[0004] Conventional starch-flavor composites have low encapsulation rates and are difficult to achieve sustained flavor release during storage and post-processing. [Means for solving the problem]
[0005] In order to solve the above problems, the present invention combines starches with different polymerization degrees with different flavor molecules to obtain various V-type crystalline starches, and realizes the sustained release of flavor during storage and post-processing of starch-based foods by controlling the crystallinity. The V-type crystalline starch of the present invention is compounded with flavor molecules, so it can be used as a starch-based seasoning in various foods.
[0006] The present invention uses starch as a raw material, and uses dry heat amorphization technology instead of conventional thermal gelatinization to thoroughly decluster starch to obtain high-concentration starch, thereby improving classification efficiency, and then obtains classified starch with different degrees of polymerization by alcohol precipitation and classification. Next, flavor molecules with different chain lengths and functional groups are selected as target substances. In the acidic solvent environment of plasma activated water, amylose with high content, high fluidity, and high solubility has more single-helix cavities, providing more sites for capturing target substances, and combined with frequency-variable ultrasound, it increases the dispersion and contact opportunities of flavor molecules in starch milk, and promotes the recombination of starch crystallization regions, thereby obtaining V-type crystalline starch with higher crystallinity, larger microcrystal size, and more densely and regularly arranged single helices.
[0007] The method of the present invention is 6I -, V 6II -, V 6III The present invention can effectively improve the crystalline structure and crystallinity of V1-, V2- and V3-type crystalline starch, and also significantly improve the encapsulation rate and sustained-release effect of various flavor molecules compared with the conventional technology, thereby significantly enhancing the practical use value of the product and providing a new technology for preserving the flavor of starch-based foods, which is an advanced version of the conventional technology of encapsulating and sustained-release of flavor molecules.
[0008] The first object of the present invention is to (1) a step of amorphization treatment in which the high amylose starch is subjected to a dry heat amorphization treatment at 130 to 135°C for 10 to 12 minutes to obtain amorphized starch; Amorphous starch and water are mixed to prepare a high-concentration starch milk of 30% to 40% by mass. Anhydrous ethanol is added to the starch milk so that the volume ratio of anhydrous ethanol to starch milk is 80% to 85%, 70% to 75%, and 55% to 60%, respectively. The mixture is then kept at 40 to 60°C for 30 to 40 minutes, and the alcohol precipitation product is separated to produce GS with different polymerization degrees. V6 , G.S. V7 , G.S. V8 (2) alcohol precipitation and classification step to obtain classified starch; GS using plasma activated water V6 , G.S. V7 , G.S. V8 The classified starches were each prepared into starch milk at 5% to 7% by mass, and then aqueous solutions of 1-decanol, 4,5-octanedione, and δ-decalactone were added to the prepared GS V6 GS was mixed with starch milk to prepare an aqueous solution of 2-acetylpyridine. V7 GS was mixed with starch milk to prepare an aqueous solution of α-pinene. V8 (3) a compounding step of mixing the starch milk with the starch milk to obtain a compound milk, sealing the compound milk, and subjecting the compound milk to variable frequency ultrasonic treatment to obtain a compound milk after variable frequency ultrasonic treatment; and (4) a cooling and crystallization step, in which the composite milk after the variable frequency ultrasonic treatment is rapidly cooled to 3-5°C at an average cooling rate of 5-10°C / min, crystallized at this temperature for 20-40 minutes, and then transferred to an environment of 20-30°C for crystallization for 2-4 hours, followed by centrifuging, washing, drying and sieving to obtain V-type crystalline starch composited with flavor molecules.
[0009] In one embodiment of the present invention, the high amylose in step (1) includes, but is not limited to, high amylose corn starch and high amylose rice starch, and the amylose content in the high amylose is 50% or more.
[0010] In one embodiment of the present invention, the dry heat amorphization treatment in step (1) is to destroy starch crystals by high-temperature dry heat technology and make the starch gelatinization degree 90% or more.
[0011] In the present invention, in step (2), different volume ratios of anhydrous ethanol and starch milk can produce classified starches with different polymerization degree ranges, resulting in three parallel schemes.
[0012] In one embodiment of the present invention, the alcohol precipitation and classification in step (2) is carried out to obtain GS having different polymerization degrees. V6 , G.S. V7 , G.S. V8 It is for obtaining classified starch, which is advantageous for the formation of V-shaped crystals with different sizes of single helical cavities, and said GS V6 , G.S. V7 , G.S. V8 The degrees of polymerization of the classified starches are 10-20, 25-35, and 40-60, respectively.
[0013] In one embodiment of the present invention, in the method for producing plasma activated water in step (3), distilled water is placed in a cylindrical tube having a diameter of 2.7 cm and a height of 12 cm, and activated for 30 to 60 s by an atmospheric pressure plasma jet device under conditions where the gas distance between the plasma jet probe and the water surface is 25 mm, to obtain plasma activated water with a pH of 5 to 6.
[0014] In the present invention, in step (3), when different flavor molecule aqueous solutions (1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, α-pinene) are used, different composite milks are obtained, and five parallel schemes are obtained. Among them, when the aqueous solutions of 1-decanol, 4,5-octanedione or δ-decalactone are used, GS V6 When starch-complex milk is obtained and later cooled and crystallized, V 6I -, V 6II -, V 6III -type crystalline starch is obtained, respectively, and when an aqueous solution of 2-acetylpyridine is used, GS V7 When a starch complex milk is obtained and later cooled and crystallized, V7-type crystalline starch is obtained, and when an aqueous solution of α-pinene is used, GS V8 A starch complex milk is obtained, which is later cooled and crystallized to obtain a V8-type crystalline starch.
[0015] In the present invention, the aqueous solutions of 1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, and α-pinene refer to dispersions of these substances, that is, dispersions in which these substances are added to water and mixed uniformly, and may be mixed by any method such as vortex mixing, high-speed stirring mixing, and ultrasonic mixing.
[0016] In one embodiment of the present invention, in the aqueous solutions of 1-decanol, 4,5-octanedione, and δ-decalactone, the aqueous solution of 2-acetylpyridine, and the aqueous solution of α-pinene in step (3), the mass ratio of 1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, and α-pinene to water is 5 to 10 mg:1 mL, and a specific production method is to uniformly disperse 1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, and α-pinene in water at 70 to 90° C. for 10 to 15 minutes.
[0017] In one embodiment of the present invention, the aqueous solution of 1-decanol, 4,5-octanedione, and δ-decalactone in step (3) and the GS V6 The volume ratio of starch milk was 0.08-0.10:1, and the aqueous solution of 2-acetylpyridine and the prepared GS V7 The volume ratio of starch milk was 0.08-0.12:1, and the aqueous solution of α-pinene and the prepared GS V8 The volume ratio to starch milk is 0.10-0.12:1.
[0018] In one embodiment of the present invention, the sealing in step (3) is sealing in a PAPE vacuum packaging bag (nylon-polyethylene composite bag).
[0019] In one embodiment of the present invention, the variable frequency ultrasonic treatment in step (3) is performed with ultrasonic frequencies of 20 to 40, 40 to 60, and 60 to 80 kHz for 20 to 30, 10 to 20, and 0 to 10 minutes, respectively, with an on-off interval of 10 to 30 seconds.
[0020] In one embodiment of the present invention, the device used for the variable frequency ultrasonic treatment in step (3) has an output of 600 W and a temperature of 70 to 90°C.
[0021] In one embodiment of the present invention, the centrifugation in step (4) comprises centrifuging at 5000×g for 15 minutes and collecting the precipitate.
[0022] In one embodiment of the present invention, the washing in step (4) is washing with ethanol.
[0023] In one embodiment of the present invention, the drying in step (4) is drying at 45 to 50° C. for 10 to 12 hours.
[0024] The second object of the present invention is to prepare V-type crystalline starch complexed with flavor molecules by the method of the present invention.
[0025] In one embodiment of the present invention, the V-type crystalline starch is 6I -, V 6II -, V 6III -, V7-, and V8-type crystalline starch.
[0026] A third object of the present invention is the use of the V-type crystalline starch complexed with said flavor molecules of the present invention in the food sector.
[0027] A fourth object of the present invention is to a step (1) of amorphization treatment, in which the high amylose is subjected to dry heat amorphization treatment at 130-135°C for 10-12 minutes to obtain amorphized starch; Amorphous starch and water are mixed to prepare a high-concentration starch milk of 30% to 40% by mass. Anhydrous ethanol is added to the starch milk so that the volume ratio of anhydrous ethanol to starch milk is 80% to 85%, 70% to 75%, and 55% to 60%, respectively. The mixture is then kept at 40 to 60°C for 30 to 40 minutes, and the alcohol precipitation product is separated to produce GS with different polymerization degrees. V6 , G.S. V7 , G.S. V8 (2) alcohol precipitation and classification step to obtain classified starch; GS using plasma activated water V6 , G.S. V7 , G.S. V8 The classified starches were each prepared into starch milk at 5% to 7% by mass, and then aqueous solutions of 1-decanol, 4,5-octanedione, and δ-decalactone were added to the prepared GS V6 GS was mixed with starch milk to prepare an aqueous solution of 2-acetylpyridine. V7 GS was mixed with starch milk to prepare an aqueous solution of α-pinene. V8 (3) a compounding step of mixing the starch milk with the starch milk to obtain a compound milk, sealing the compound milk, and subjecting the compound milk to variable frequency ultrasonic treatment to obtain a compound milk after variable frequency ultrasonic treatment; and (4) a cooling and crystallization step, in which the compound milk after variable frequency ultrasonic treatment is rapidly cooled to 3-5°C at an average cooling rate of 5-10°C / min, crystallized at this temperature for 20-40 minutes, and then transferred to an environment of 20-30°C for crystallization for 2-4 hours, followed by centrifuging, washing, drying and sieving to obtain V-type crystalline starch compounded with flavor molecules.
[0028] The fifth object of the present invention is to 6I -, V 6II -, V 6III The present invention also provides a seasoning containing the V-type crystalline starch of the present invention, which contains one or more of V-, V7-, or V8-type crystalline starch.
[0029] The seasoning may be added to the food in an amount within the range permitted by local law, the amount being the flavor molecular weight of V-type crystalline starch converted.
[0030] In one embodiment, the V-type crystalline starch is V-type crystalline starch complexed with 1-decanol. 6I V-type crystalline starch can be used in rice and flour products, baked goods, confectionery, and other foods. The V-type crystalline starch is a V-type crystalline starch complexed with 4,5-octanedione. 6IIIt is a V-type crystalline starch that can be used in foods such as rice and flour products, baked goods, and confectioneries. The V-type crystalline starch is a V-type crystalline starch complexed with δ-decalactone. 6III The V-type crystalline starch is a V7-type crystalline starch complexed with 2-acetylpyridine, which can be used in foods such as rice and flour products, nuts, confectioneries, and baked goods. The V-type crystalline starch is a V8-type crystalline starch complexed with α-pinene, which can be used in foods such as soft drinks, cold drinks, and baked goods.
[0031] In the present invention, the flavour molecules are: (1) 1-Decanol: It has a waxy, sweet, floral or fruity scent. According to GB 2760-2014, it is permitted to be added as a flavoring in an appropriate amount required for manufacturing, and can be used in foods such as rice and flour products, baked goods, confectionery, and beverages. (2) 4,5-octanedione: It has a creamy fragrance and is permitted to be added as a flavoring in an appropriate amount according to GB 2760-2014, and can be used in foods such as rice and flour products, baked goods, and confectioneries. (3) δ-Decalactone: It has a fruity scent like coconut and peach, and at low concentrations it has a creamy scent. According to GB 2760-2014, it is permitted to be added as a flavoring in an appropriate amount required for manufacturing, and can be used in foods such as dairy products, soft drinks, cold drinks, confectioneries, and baked goods. (4) 2-Acetylpyridine: It has a popcorn or nutty aroma and can be used as a flavoring in rice and flour products, confectionery, nuts, baked goods, etc. according to GB 2760-2014. (5) α-pinene: It has a refreshing pine-like scent. According to GB 2760-2014, it is permitted to be added as a flavoring in an appropriate amount required for manufacturing, and can be used in foods such as soft drinks, cold drinks, and baked goods. Effect of the Invention
[0032] (1) In the present invention, starch is sufficiently declustered by dry heat amorphization, the degree of gelatinization of starch is increased to 90% or more, the starch concentration is effectively increased, and the production efficiency of classified starch is significantly improved. (2) In the present invention, classified starches with different polymerization degrees can be obtained by alcohol precipitation and classification, and starch raw materials suitable for forming V-shaped crystals with different sizes of single helical cavities can be obtained. (3) In the present invention, the plasma activated water is used to provide an acidic solvent environment, which enhances the fluidity of starch chains, improves the solubility of starch, and provides more sites for capturing target molecules through more single helical cavities. In addition, by combining with the frequency-variable ultrasound-assisted complexation method, it is possible to obtain a high encapsulation rate and sustained release effect for flavor molecules. 6I -, V 6II -, V 6III V-, V7-, and V8-type crystalline starch can be obtained. The V-type crystalline starch composited by combining plasma activated water and frequency-variable ultrasound has significantly improved short-range order and crystallinity, and such an ordered crystalline structure is advantageous in stabilizing the flavor molecules embedded therein and increasing resistance to environmental changes. (4) In the present invention, a large amount of crystal nuclei are formed by the rapid cooling and crystallization method, and the growth of crystals is promoted by keeping the temperature at an appropriate level, which is advantageous for further crystallization of the V-type crystalline starch complexed with flavor molecules and for further enlarging the size of the microcrystals, and the crystal structure tends to be complete, which is advantageous for extending the release time of the flavor molecules in the complex and improving the stability of the complex. (5) In the present invention, the embedding and sustained-release effects of flavor molecules in V-type crystalline starch complexed with flavor molecules were further tested. The test results showed that when flavor molecules are adsorbed and embedded in starch milk that has been subjected to normal hydrothermal treatment, the maximum adsorption rate is 8.2%, while the V-type crystalline starch complexed with flavor molecules produced in the present invention has a maximum embedding rate of 68.2%. Flavor molecules complexed with various V-type crystalline starches have significantly improved embedding rates and sustained-release effects, and all types of V-type crystals are suitable for embedding and controlled release of various flavor molecules. (6) The present invention uses various flavor molecules to form various crystalline starches, and then realizes the sustained release of flavor during storage and post-processing by controlling the crystallization properties. The obtained V-type crystalline starch complexed with flavor molecules has a significantly improved embedding rate and sustained release effect of flavor molecules compared to conventional techniques, making it possible to provide a new technique for preserving the flavor of starch-based foods. This is an advanced version of the conventional flavor molecule embedding and sustained release technique, and the V-type crystalline starch can also be added to starch-based foods as a compounding ingredient to improve the flavor of the food, which is expected to add industrial added value. [Brief description of the drawings]
[0033] [Figure 1] 4 shows the effect of various flavor molecules selected in Examples 1 to 5 on starch crystal form. [Diagram 2] The effects of various treatment methods on the V6I-type crystal structure: A: dry heat amorphization treatment (Scheme 6 in Comparative Example 2) alone, B: dry heat amorphization + alcohol precipitation / classification (Scheme 3 in Comparative Example 2), C: dry heat amorphization + alcohol precipitation / classification + plasma activated water + variable frequency ultrasonic (Example 1). DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0034] Preferred embodiments of the present invention will now be described. It should be understood that the embodiments are provided for the purpose of better illustrating the present invention and are not intended to limit the present invention.
[0035] Test Method 1. Test method for embedding rate of flavor molecules (1) Measurement of calibration curve: Add an appropriate amount of flavor molecules to absolute ethanol to obtain flavor molecule absolute ethanol solutions of 0.1, 0.2, 0.3, 0.4, 0.5, and 0.6 μL / mL. Obtain the corresponding peak area by gas chromatography analysis, and obtain the corresponding regression equation with the volume concentration of the flavor molecules as the abscissa and the peak area of the measured flavor molecules as the ordinate. (2) Determination of the content of flavor molecules in the composite: Accurately weigh 20 mg of V-type crystalline starch complexed with flavor molecules, add 5 mL of absolute ethanol, seal and mix uniformly, and ultrasonicate at 60°C for 30 minutes to transfer the flavor molecules from the cavity of the V-type crystals to absolute ethanol. Obtain the corresponding peak area by gas chromatography analysis, and calculate the content of flavor molecules in the composite using a regression equation. The formula for calculating the embedding rate is shown in the following formula (1). Encapsulation rate % = number of moles of flavor molecules in the composite (mol) / number of moles of flavor molecules initially added (mol) × 100 (1) Gas chromatography conditions: DB-WAX chromatographic column (length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm); inlet temperature: 200 ° C; detector temperature: 250 ° C; carrier gas: nitrogen, flow rate 3.0 mL / min. Gas chromatography measurement procedure: Initial temperature is 35 ° C, kept for 5 min, then heated to 180 ° C at a rate of 5 ° C / min, heated from 180 ° C to 250 ° C at a rate of 10 ° C / min, and kept for 5 min. 2. Testing the sustained release effect of flavor ingredients The composite was placed in an environment of 20°C and 12% relative humidity, and at 96 h, 240 h, and 720 h, the same amount of composite (5.0 g) was sampled and quickly transferred to a 20 mL headspace vial, and the headspace concentration of each flavor molecule was measured by gas chromatography. Gas chromatography conditions: DB-WAX chromatographic column (length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm); inlet temperature: 200 °C; detector temperature: 250 °C; carrier gas: nitrogen, flow rate 3.0 mL / min. Gas chromatography measurement procedure: Initial temperature is 35 °C, kept for 5 min, then heated to 180 °C at a rate of 5 °C / min, heated from 180 °C to 250 °C at a rate of 10 °C / min, and kept for 5 min.
[0036] Example 1 V with flavor molecules 6I A method for producing crystalline starch, comprising the steps of: (1) Amorphization treatment High amylose cornstarch (amylose content 80%) was subjected to dry heat amorphization treatment at 135℃ for 12 minutes to obtain amorphized starch. (2) Alcohol precipitation and classification Amorphous starch and water were mixed to prepare a high-concentration starch milk of 35% by mass, and absolute ethanol was added to the starch milk so that the volume ratio of absolute ethanol to starch milk was 80%. The mixture was then kept at 50°C for 30 minutes, and the alcohol precipitation product was separated to obtain GS with a degree of polymerization of 10 to 20. V6 Starch was obtained. (3) Compounding Distilled water was placed in a cylindrical tube with a diameter of 2.7 cm and a height of 12 cm, and activated for 30 s with an atmospheric pressure plasma jet device under the condition that the gas distance between the plasma jet probe and the water surface was 25 mm, to obtain plasma activated water with a pH of 6. GS using plasma activated water V6 Starch was prepared into 6% by mass starch milk, and then 10 mL of a 1-decanol aqueous solution having a concentration of 10 mg / mL (i.e., a dispersion of 1-decanol, which may be prepared by adding 1-decanol to water and uniformly mixing it by vortex mixing) was added to the prepared GS V6 The mixture was mixed with 100 mL of starch milk to obtain mixed milk. The mixed milk was then placed in a PAPE vacuum packaging bag (nylon-polyethylene composite bag) and sealed. Next, ultrasonic waves with frequencies of 20, 40, and 60 kHz were applied to the sealed and packaged mixed milk for 30, 20, and 10 min, with an on-off interval of 30 s, an output of the device used for frequency-variable ultrasonic treatment of 600 W, and a temperature of 80°C, to obtain composite milk after frequency-variable ultrasonic treatment. (4) Cooling and crystallization The composite milk after variable frequency ultrasonic treatment was rapidly cooled to 4°C with an average cooling rate of 8°C / min, crystallized at this temperature for 30 min, and then transferred to an environment of 25°C for crystallization for 3 h. After cooling and crystallization, it was centrifuged at 5000×g for 15 min, and the precipitate was collected, washed with absolute ethanol three times, dried, and sieved to obtain the flavor molecule-complexed V. 6I -type crystalline starch was obtained.
[0037] Example 2 V with flavor molecules 6IIA method for producing crystalline starch, comprising the steps of: (1) Amorphization treatment High amylose cornstarch (amylose content 80%) was subjected to dry heat amorphization treatment at 135℃ for 12 minutes to obtain amorphized starch. (2) Alcohol precipitation and classification Amorphous starch and water were mixed to prepare a high-concentration starch milk of 35% by mass, and absolute ethanol was added to the starch milk so that the volume ratio of absolute ethanol to starch milk was 80%. The mixture was then kept at 50°C for 30 minutes, and the alcohol precipitation product was separated to obtain GS with a degree of polymerization of 10 to 20. V6 Starch was obtained. (3) Compounding Distilled water was placed in a cylindrical tube with a diameter of 2.7 cm and a height of 12 cm, and activated for 30 s using an atmospheric pressure plasma jet device with a gas distance of 25 mm between the plasma jet probe and the water surface to obtain plasma-activated water with a pH of 6. GS using plasma activated water V6 Starch was prepared into 6% by mass starch milk, and then 10 mL of a 10 mg / mL aqueous solution of 4,5-octanedione (i.e., a dispersion of 4,5-octanedione, which may be prepared by adding 4,5-octanedione to water and mixing uniformly with a vortex) was prepared. V6 The mixture was mixed with 100 mL of starch milk to obtain mixed milk. The mixed milk was then placed in a PAPE vacuum packaging bag (nylon-polyethylene composite bag) and sealed. Next, ultrasonic waves with frequencies of 20, 40, and 60 kHz were applied to the sealed and packaged mixed milk for 30, 20, and 10 min, with an on-off interval of 30 s, an output of the device used for frequency-variable ultrasonic treatment of 600 W, and a temperature of 80°C, to obtain composite milk after frequency-variable ultrasonic treatment. (4) Cooling and crystallization The composite milk after variable frequency ultrasonic treatment was rapidly cooled to 4°C with an average cooling rate of 8°C / min, crystallized at this temperature for 30 min, and then transferred to an environment of 25°C for crystallization for 3 h. After cooling and crystallization, it was centrifuged at 5000×g for 15 min, and the precipitate was collected, washed with absolute ethanol three times, dried, and sieved to obtain the flavor molecule-complexed V. 6II -type crystalline starch was obtained.
[0038] Example 3 V with flavor molecules 6III A method for producing crystalline starch, comprising the steps of: (1) Amorphization treatment High amylose cornstarch (amylose content 80%) was subjected to dry heat amorphization treatment at 135℃ for 12 minutes to obtain amorphized starch. (2) Alcohol precipitation and classification Amorphous starch and water were mixed to prepare a high-concentration starch milk of 35% by mass, and absolute ethanol was added to the starch milk so that the volume ratio of absolute ethanol to starch milk was 80%. The mixture was then kept at 50°C for 30 minutes, and the alcohol precipitation product was separated to obtain GS with a degree of polymerization of 10 to 20. V6 Starch was obtained. (3) Compounding Distilled water was placed in a cylindrical tube with a diameter of 2.7 cm and a height of 12 cm, and activated for 30 s using an atmospheric pressure plasma jet device with a gas distance of 25 mm between the plasma jet probe and the water surface to obtain plasma-activated water with a pH of 6. GS using plasma activated water V6 Starch was prepared as 6% by mass starch milk, and then 10 mL of a 10 mg / mL δ-decalactone aqueous solution was prepared. V6 The mixture was mixed with 100 mL of starch milk to obtain mixed milk. The mixed milk was then placed in a PAPE vacuum packaging bag (nylon-polyethylene composite bag) and sealed. Next, ultrasonic waves with frequencies of 20, 40, and 60 kHz were applied to the sealed and packaged mixed milk for 30, 20, and 10 min, with an on-off interval of 30 s, an output of the device used for frequency-variable ultrasonic treatment of 600 W, and a temperature of 80°C, to obtain composite milk after frequency-variable ultrasonic treatment. (4) Cooling and crystallization The composite milk after variable frequency ultrasonic treatment was rapidly cooled to 4°C with an average cooling rate of 8°C / min, crystallized at this temperature for 30 min, and then transferred to an environment of 25°C for crystallization for 3 h. After cooling and crystallization, it was centrifuged at 5000×g for 15 min, and the precipitate was collected, washed with absolute ethanol three times, dried, and sieved to obtain the flavor molecule-complexed V. 6III-type crystalline starch was obtained.
[0039] Example 4 A method for preparing V7-type crystalline starch complexed with flavor molecules, comprising the steps of: (1) Amorphization treatment High amylose cornstarch (amylose content 80%) was subjected to dry heat amorphization treatment at 135℃ for 12 minutes to obtain amorphized starch. (2) Alcohol precipitation and classification Amorphous starch and water were mixed to prepare a high-concentration starch milk of 35% by mass, and absolute ethanol was added to the starch milk so that the volume ratio of absolute ethanol to starch milk was 75%. The mixture was then kept at 50°C for 40 minutes, and the alcohol precipitation product was separated to obtain GS with a degree of polymerization of 25 to 35. V7 Starch was obtained. (3) Compounding Distilled water was placed in a cylindrical tube with a diameter of 2.7 cm and a height of 12 cm, and activated for 30 s using an atmospheric pressure plasma jet device with a gas distance of 25 mm between the plasma jet probe and the water surface to obtain plasma-activated water with a pH of 6. GS using plasma activated water V7 Starch was prepared as 6% by mass starch milk, and then 10 mL of 2-acetylpyridine aqueous solution with a concentration of 10 mg / mL was prepared. V7 The mixture was mixed with 100 mL of starch milk to obtain mixed milk. The mixed milk was then placed in a PAPE vacuum packaging bag (nylon-polyethylene composite bag) and sealed. Next, ultrasonic waves with frequencies of 20, 40, and 60 kHz were applied to the sealed and packaged mixed milk for 30, 20, and 10 min, with an on-off interval of 30 s, an output of the device used for frequency-variable ultrasonic treatment of 600 W, and a temperature of 80°C, to obtain composite milk after frequency-variable ultrasonic treatment. (4) Cooling and crystallization The composite milk after variable frequency ultrasonic treatment was rapidly cooled to 4°C at an average cooling rate of 8°C / min, crystallized at this temperature for 30 min, and then transferred to an environment of 25°C for crystallization for 3 h. After cooling and crystallization, it was centrifuged at 5000×g for 15 min, and the precipitate was collected, washed with absolute ethanol three times, dried and sieved to obtain flavor molecule-complexed V7-type crystalline starch.
[0040] Example 5 A method for preparing V8-type crystalline starch complexed with flavor molecules, comprising the steps of: (1) Amorphization treatment High amylose cornstarch (amylose content 80%) was subjected to dry heat amorphization treatment at 135℃ for 12 minutes to obtain amorphized starch. (2) Alcohol precipitation and classification Amorphous starch and water were mixed to prepare a high-concentration starch milk of 35% by mass, and absolute ethanol was added to the starch milk so that the volume ratio of absolute ethanol to starch milk was 60%. The mixture was then kept at 60°C for 40 minutes, and the alcohol precipitation product was separated to obtain GS with a degree of polymerization of 40 to 60. V8 Starch was obtained. (3) Compounding Distilled water was placed in a cylindrical tube with a diameter of 2.7 cm and a height of 12 cm, and activated for 30 s using an atmospheric pressure plasma jet device with a gas distance of 25 mm between the plasma jet probe and the water surface to obtain plasma-activated water with a pH of 6. GS using plasma activated water V8 Starch was prepared as 6% by mass starch milk, and then 10 mL of an aqueous solution of α-pinene with a concentration of 10 mg / mL was prepared. V8 The mixture was mixed with 100 mL of starch milk to obtain mixed milk. The mixed milk was then placed in a PAPE vacuum packaging bag (nylon-polyethylene composite bag) and sealed. Next, ultrasonic waves with frequencies of 20, 40, and 60 kHz were applied to the sealed and packaged mixed milk for 30, 20, and 10 min, with an on-off interval of 30 s, an output of the device used for frequency-variable ultrasonic treatment of 600 W, and a temperature of 80°C, to obtain composite milk after frequency-variable ultrasonic treatment. (4) Cooling and crystallization The composite milk after variable frequency ultrasonic treatment was rapidly cooled to 4°C at an average cooling rate of 8°C / min, crystallized at this temperature for 30 min, and then transferred to an environment of 25°C for crystallization for 3 h. After cooling and crystallization, it was centrifuged at 5000×g for 15 min, and the precipitate was collected, washed with absolute ethanol three times, dried and sieved to obtain flavor molecule-complexed V8-type crystalline starch. The V-type crystalline starches obtained in Examples 1 to 5 were subjected to performance tests, and the test results are shown below. As can be seen from Table 1, among the five types of V-type crystalline starch, the highest encapsulation rate of flavor molecules was 68.2%, and the lowest was 65.4%. In an environment of 20°C and 12% relative humidity, the release of flavor molecules was confirmed for all composites at the detection time of 720 h. [Table 1] TIFF0007642082000001.tif42170 Figure 1 shows the effect of various flavor molecules selected in Examples 1 to 5 on the crystal form of starch. As can be seen from Figure 1, different flavor molecules cause different V-type crystal structures to be formed in starch.
[0041] Example 6 The amorphous starch and water in step (2) of Examples 1 to 3 were prepared into a high-concentration starch milk of 40% by mass, and the volume ratio of anhydrous ethanol to starch milk was 85%. In step (3), the pH of the plasma activated water was 5, the concentration of the starch milk was 5%, and the ultrasonic application time was 20, 10, and 0 minutes. The rest was the same as in Examples 1 to 3, and V complexed with flavor molecules was prepared. 6I -Type, V 6II -type and V 6III -type crystalline starch was obtained. A high-concentration starch milk was prepared by mixing the amorphous starch and water in step (2) of Example 4 at 40% by mass, and the volume ratio of anhydrous ethanol to starch milk was 70%. In step (3), the pH of the plasma activated water was 5, the concentration of the starch milk was 5%, and the ultrasonic application time was 20, 10, and 0 min. The rest of the procedure was the same as in Example 4, and a V7-type crystalline starch complexed with flavor molecules was obtained. In step (2) of Example 5, the anhydrous ethanol and starch milk were kept at 40°C for 40 minutes. In step (3), the pH of the plasma activated water was 5, the concentration of the starch milk was 5%, and the ultrasonic application time was 20, 10, and 0 minutes. The rest was the same as in Example 5 to obtain a V8-type crystalline starch complexed with flavor molecules. The V-type crystalline starch was subjected to performance tests, and the test results are shown below. As can be seen from Table 2, among the five types of V-type crystalline starch, the highest encapsulation rate of flavor molecules was 65.1%, and the lowest was 62.7%. In an environment of 20°C and 12% relative humidity, the release of flavor molecules was confirmed for all composites at the detection time of 720 h. [Table 2] TIFF0007642082000002.tif42170
[0042] Example 7 The temperature of the amorphization treatment in step (1) of Examples 1 to 3 was 130°C. In step (3), the concentration of starch milk was 7%, and the temperature in the variable frequency ultrasonic treatment was 90°C. In step (4), the cooling and crystallization was performed by rapidly cooling to 3°C at an average cooling rate of 5°C / min, crystallizing at this temperature for 20 min, and then transferring to an environment of 20°C for crystallization for 2 h. Other than that, the V complexed with flavor molecules was prepared in the same manner as in Examples 1 to 3. 6I -Type, V 6II -type and V 6III -type crystalline starch was obtained. In step (1) of Example 4, the amorphization treatment temperature was 130°C. In step (2), amorphized starch and water were prepared into a high-concentration starch milk of 30% by mass. In step (3), the concentration of starch milk was 7% by mass, and the temperature in the variable frequency ultrasonic treatment was 90°C. In step (4), the cooling and crystallization involved rapid cooling to 3°C at an average cooling rate of 5°C / min, crystallization at this temperature for 20 minutes, and then transferring to an environment of 20°C for crystallization for 2 hours. Other than that, the remainder was the same as in Example 4 to obtain a V7-type crystalline starch complexed with flavor molecules. In step (1) of Example 5, the amorphization treatment temperature was 130°C. In step (2), a high-concentration starch milk containing 30% amorphized starch and water was prepared, and the volume ratio of anhydrous ethanol to starch milk was 55%. In step (3), the concentration of starch milk was 7% by mass, and the variable frequency ultrasonic treatment used ultrasonic waves with frequencies of 40, 60, and 80 kHz. In step (4), the cooling and crystallization was performed by rapidly cooling to 3°C at an average cooling rate of 5°C / min, crystallizing at this temperature for 20 minutes, and then transferring to an environment of 20°C for crystallization for 2 hours. Other than that, the remaining steps were the same as in Example 5 to obtain a flavor molecule-complexed V8-type crystalline starch. The V-type crystalline starch was subjected to performance tests, and the test results are shown below. As can be seen from Table 3, among the five types of V-type crystalline starch, the highest encapsulation rate of flavor molecules reached 66.9% and the lowest was 64.2%. In an environment of 20°C and 12% relative humidity, the release of flavor molecules was confirmed for all composites at the detection time of 720 h. [Table 3] TIFF0007642082000003.tif42170
[0043] Comparative Example 1 A method for preparing V-type crystalline starch complexed with flavor molecules, comprising the steps of: (1) Using deionized water, high amylose cornstarch (amylose content 80%) was prepared into starch milk with a starch dry weight of 6%, which was then placed in a boiling water bath and stirred for 90 minutes while being heated to obtain gelatinized starch milk. (2) 100 mL of gelatinized starch milk was quickly cooled to 80°C and mixed with 10 mL of aqueous solutions of flavor compounds (1-decanol aqueous solution with a concentration of 10 mg / mL, 4,5-octanedione aqueous solution with a concentration of 10 mg / mL, δ-decalactone aqueous solution with a concentration of 10 mg / mL, 2-acetylpyridine aqueous solution with a concentration of 10 mg / mL, and α-pinene aqueous solution with a concentration of 10 mg / mL) to obtain mixed milk, which was sealed and reacted for 20 min under stirring at 80°C. The composite milk was then cooled, stored at room temperature for 24 h, centrifuged at 5000×g for 15 min, the precipitate was collected, washed with anhydrous ethanol three times, and baked to obtain V-type crystalline starch with various structures. The obtained V-type crystalline starch was subjected to performance tests, and the test results are shown below. As can be seen from Table 4, among the five types of V-type crystalline starches, the highest embedding rate of flavor molecules was only 8.2%. At 20°C and 12% relative humidity, no flavor molecules were detected in any of the composites after 96 h. [Table 4] TIFF0007642082000004.tif42170Comparing Examples 1 to 5 with Comparative Example 1, the samples produced without using dry heat amorphization, alcohol precipitation and classification, and the combination of plasma activated water and frequency variable ultrasound had a low embedding rate of flavor molecules, and the release rate of flavor molecules during the complex was fast under room temperature and dry storage conditions, which is unfavorable for application in the food industry. Compared with Comparative Example 1, the methods of Examples 1 to 5 significantly improved the adsorption rate of flavor molecules and the release time under room temperature and dry storage conditions. By thoroughly declustering starch by dry heat amorphization and then performing alcohol precipitation and classification, various suitable classified starches formed with V-type crystals were obtained. In the favorable solvent environment of plasma-activated water, amylose is easy to separate from the particles and diffuse, which increases the solubility of starch, and the hydrolysis of acidic substances in plasma-activated water promotes the flow of starch, providing more sites for capturing target molecules; and, combined with the assisted action of frequency-variable ultrasound, flavor molecules are more easily able to interact with the interface between the internal cavities of amorphous granular starch and enter the cavities, resulting in V-type crystalline starch with more embedded flavor molecules and larger crystallinity and crystallite size. After treatment, the V-type crystals tend to have improved short-range order and crystallinity, and a complete crystal structure. Such an ordered crystal structure is favorable for stabilizing the embedded flavor molecules and increasing the resistance to environmental changes, and can extend the release time of the flavor molecules in the composite and increase the stability of the composite. In this way, the purpose of effective embedding and sustained release of flavor molecules in starch-based products is achieved.
[0044] Comparative Example 2 Scheme 1: V, which is a conjugated flavor molecule, was prepared in the same manner as in Example 1, except that step (1) in Example 1 was omitted and high amylose cornstarch and water were directly heated and gelatinized. 6I -type crystalline starch was obtained. Scheme 2: Step (2) in Example 1 was omitted, and high amylose cornstarch and plasma activated water were directly mixed to produce starch milk. The rest of the procedure was the same as in Example 1, and flavor molecule-complexed V 6I -type crystalline starch was obtained. Scheme 3: V complexed with flavor molecules was prepared in the same manner as in Example 1, except that the plasma activated water in step (3) of Example 1 was replaced with deionized water and ultrasonic treatment was not performed. 6I -type crystalline starch was obtained. Scheme 4: Steps (1) and (2) of Example 1 were omitted, and high amylose corn starch and plasma activated water were directly prepared into starch milk. The rest was the same as in Example 1, and flavor molecule-complexed V 6I -type crystalline starch was obtained. Scheme 5: By omitting steps (1) and (3) of Example 1, high amylose cornstarch and water were directly heated and gelatinized to obtain GS with a degree of polymerization of 10 to 20. V6 The remaining process was the same as in Example 1 except that the starch was obtained, then mixed with water to produce starch milk, then sealed, cooled and crystallized, centrifuged, washed and dried, and the V complexed with flavor molecules was obtained. 6I -type crystalline starch was obtained. Scheme 6: The steps (2) and (3) of Example 1 were omitted, and the amorphized starch obtained in step (1) was mixed with water to prepare starch milk, which was then sealed, cooled and crystallized, centrifuged, washed and dried. The rest of the procedure was the same as in Example 1 to prepare V complexed with flavor molecules. 6I -type crystalline starch was obtained. The conditions for Schemes 1 to 6 are shown below. [Table 5] Operating conditions TIFF0007642082000005.tif53170 Note: "+" indicates that the operation is performed, and "-" indicates that the operation is not performed. The remaining operation conditions are all the same as those in the scope of the present invention. The V-type crystalline starch thus obtained was subjected to performance tests, and the test results are shown below. As can be seen from Table 6, the encapsulation rate and sustained release effect of flavor molecules could not be obtained by either dry heat amorphization, alcohol precipitation / classification, or plasma activated water + frequency-variable ultrasound alone, or by a combination of two of dry heat amorphization, alcohol precipitation / classification, or plasma activated water + frequency-variable ultrasound, and only a combination of the three of them produced starch with a high encapsulation rate and sustained release effect of flavor molecules. In addition, the three methods of dry heat amorphization, alcohol precipitation / classification, and plasma activated water + frequency-variable ultrasound have a synergistic effect. [Table 6] TIFF0007642082000006.tif54170Note: "√" indicates that the flavor molecule was identified, and "×" indicates that the flavor molecule was not identified. Figure 2 shows the various processing methods. 6I The effects on the V-type crystal structure are as follows: A: Dry heat amorphization treatment (Scheme 6 in Comparative Example 2) alone; B: Dry heat amorphization + alcohol precipitation / classification (Scheme 3 in Comparative Example 2); C: Dry heat amorphization + alcohol precipitation / classification + plasma activated water + frequency-variable ultrasonic (Example 1). As can be seen from Figure 2, only when the three techniques are combined, the crystal structure tends to be complete, and V-type crystals with a higher degree of crystallinity are obtained, which is favorable for embedding and sustained release of flavor molecules.
[0045] Comparative Example 3 Scheme 1: Step (1) of Example 4 was omitted, and high amylose corn starch and water were directly heated and gelatinized, but the rest of the procedure was the same as in Example 4 to obtain a V7-type crystalline starch complexed with flavor molecules. Scheme 2: Step (2) of Example 4 was omitted, and high amylose corn starch and plasma activated water were directly mixed to produce starch milk. The rest of the procedure was the same as in Example 4 to obtain V7-type crystalline starch complexed with flavor molecules. Scheme 3: A V7-type crystalline starch complexed with flavor molecules was obtained in the same manner as in Example 4, except that the plasma-activated water in step (3) of Example 4 was replaced with deionized water and ultrasonic treatment was not performed. Scheme 4: Steps (1) and (2) of Example 4 were omitted, and high amylose corn starch and plasma activated water were directly prepared into starch milk. The rest of the procedure was the same as in Example 4 to obtain a V7-type crystalline starch complexed with flavor molecules. Scheme 5: By omitting steps (1) and (3) of Example 4, high amylose cornstarch and water were directly heated and gelatinized to obtain GS with a degree of polymerization of 25 to 35. V7 The starch was obtained, then mixed with water to produce starch milk, which was then sealed, cooled and crystallized, centrifuged, washed and dried, but the rest was the same as in Example 4 to obtain a V7-type crystalline starch complexed with flavor molecules. Scheme 6: Steps (2) and (3) of Example 4 were omitted, and the amorphous starch obtained in step (1) was mixed with water to prepare starch milk, which was then sealed, cooled and crystallized, centrifuged, washed and dried. The rest of the procedure was the same as in Example 4 to obtain a V7-type crystalline starch complexed with flavor molecules. The conditions for Schemes 1 to 6 are shown below. [Table 7] Operating conditions TIFF0007642082000007.tif53170 Note: "+" indicates that the operation is performed, and "-" indicates that the operation is not performed. The remaining operation conditions are all within the scope of the present invention. The obtained V-type crystalline starch was subjected to performance tests, and the test results are shown below. As can be seen from Table 8, the encapsulation rate and sustained release effect of flavor molecules could not be obtained by either dry heat amorphization, alcohol precipitation / classification, or plasma activated water + variable frequency ultrasound alone, or by a combination of two of each of dry heat amorphization, alcohol precipitation / classification, or plasma activated water + variable frequency ultrasound, and only a combination of the three of them produced starch with a high encapsulation rate and sustained release effect of flavor molecules. In addition, the three of dry heat amorphization, alcohol precipitation / classification, and plasma activated water + variable frequency ultrasound have a synergistic effect. [Table 8] TIFF0007642082000008.tif54170Note: "√" indicates that the flavor molecule was identified, and "×" indicates that the flavor molecule was not identified.
[0046] Comparative Example 4 Scheme 1: Step (1) of Example 5 was omitted, and high amylose corn starch and water were directly heated and gelatinized, but the rest of the procedure was the same as in Example 5 to obtain a V8-type crystalline starch complexed with flavor molecules. Scheme 2: Step (2) of Example 5 was omitted, and high amylose corn starch and plasma activated water were directly mixed to produce starch milk. The rest of the procedure was the same as in Example 5 to obtain V8-type crystalline starch complexed with flavor molecules. Scheme 3: A V8-type crystalline starch complexed with flavor molecules was obtained in the same manner as in Example 5, except that the plasma-activated water in step (3) of Example 5 was replaced with deionized water and ultrasonic treatment was not performed. Scheme 4: Steps (1) and (2) of Example 5 were omitted, and high amylose corn starch and plasma activated water were directly prepared into starch milk. The rest of the procedure was the same as in Example 5 to obtain V8-type crystalline starch complexed with flavor molecules. Scheme 5: By omitting steps (1) and (3) of Example 5, high amylose cornstarch and water were directly heated and gelatinized to obtain GS with a degree of polymerization of 40 to 60. V8 The starch was obtained, then mixed with water to produce starch milk, then sealed, cooled and crystallized, centrifuged, washed and dried, except for the rest, which was the same as in Example 5, to obtain V8-type crystalline starch complexed with flavor molecules. Scheme 6: Steps (2) and (3) of Example 5 were omitted, and the amorphous starch obtained in step (1) was mixed with water to prepare starch milk, which was then sealed, cooled and crystallized, centrifuged, washed and dried. The rest of the procedure was the same as in Example 5 to obtain a V8-type crystalline starch complexed with flavor molecules. The conditions for Schemes 1 to 6 are shown below. [Table 9] Operating conditions TIFF0007642082000009.tif54170 Note: "+" indicates that the operation is performed, and "-" indicates that the operation is not performed. The remaining operation conditions are all within the scope of the present invention. The V-type crystalline starch thus obtained was subjected to performance tests, and the test results are shown below. As can be seen from Table 10, the encapsulation rate and sustained release effect of flavor molecules could not be achieved by either dry heat amorphization, alcohol precipitation / classification, or plasma activated water + frequency-variable ultrasound alone, or by any combination of two of dry heat amorphization, alcohol precipitation / classification, or plasma activated water + frequency-variable ultrasound, and only the combination of the three resulted in starch with a high encapsulation rate and sustained release of flavor molecules. In addition, the three methods of dry heat amorphization, alcohol precipitation / classification, and plasma activated water + frequency-variable ultrasound have a synergistic effect. [Table 10] TIFF0007642082000010.tif54170Note: "√" indicates that the flavor molecule was identified, and "×" indicates that the flavor molecule was not identified.
[0047] Example 8: Use of V-type crystalline starch as a seasoning in the processing of black rice porridge with excellent shelf life The black rice porridge has excellent shelf life, and the processing method thereof specifically includes the following steps: S1: The raw materials, brown rice and black rice, were washed and drained. S2:V 7- The black rice porridge cooking system was conditioned using V-type crystalline starch, i.e. 7- Crystalline starch, white sugar, rice, and black rice were mixed in a mass ratio of 1:1:10:10, and then water was added so that the mass ratio of rice to water was 1:1.5, and the mixture was soaked for 30 minutes. S3: Aseptically individually packaged, steamed for 30 minutes, and aseptically vacuum sealed. S4: Stored after it had cooled down.
[0048] The present invention has been disclosed above by way of preferred embodiments, but these embodiments do not limit the present invention. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and the scope of the rights of the present invention is defined by the claims.
Claims
1. A method for producing V-type crystalline starch complexed with flavor molecules, comprising: a step (1) of amorphization treatment, in which the high amylose starch is subjected to a dry heat amorphization treatment at 130-135°C for 10-12 minutes to obtain amorphized starch; Amorphous starch and water are prepared into a high-concentration starch milk of 30% to 40% by mass, and anhydrous ethanol is added to the starch milk so that the volume ratios of anhydrous ethanol to starch milk are 80% to 85%, 70% to 75%, and 55% to 60%, respectively. The mixture is then kept at 40 to 60°C for 30 to 40 minutes, and the alcohol precipitation product is separated to obtain GS having different polymerization degrees. V6 , G.S. V7 , G.S. V8 (2) a step of alcohol precipitation and classification to obtain a classified starch; Using plasma activated water, GS V6 , G.S. V7 , G.S. V8 The classified starches were each prepared into starch milk with a concentration of 5% to 7% by mass, and then aqueous solutions of 1-decanol, 4,5-octanedione, and δ-decalactone were added to the prepared GS. V6 GS was mixed with starch milk to prepare an aqueous solution of 2-acetylpyridine. V7 GS was mixed with starch milk to prepare an aqueous solution of α-pinene. V8 (3) a compounding step of mixing the starch milk with the starch milk to obtain a compound milk, sealing the compound milk, and subjecting the compound milk to variable frequency ultrasonic treatment to obtain a compound milk after variable frequency ultrasonic treatment; and (4) a cooling and crystallization step, in which the composite milk after the variable frequency ultrasonic treatment is rapidly cooled to 3-5°C at an average cooling rate of 5-10°C / min, crystallized at this temperature for 20-40 min, and then transferred to an environment of 20-30°C for crystallization for 2-4 h, followed by centrifuging, washing, drying and sieving to obtain a V-type crystalline starch composited with flavor molecules.
2. The GS of step (2) V6 , G.S. V7 , G.S. V8 The method according to claim 1, wherein the degree of polymerization of the classified starches is 10-20, 25-35, or 40-60, respectively.
3. The method according to claim 1, wherein the mass ratio of 1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, α-pinene to water in the aqueous solution of 1-decanol, 4,5-octanedione, δ-decalactone, the aqueous solution of 2-acetylpyridine, and the aqueous solution of α-pinene in step (3) is 5 to 10 mg:1 mL.
4. The aqueous solution of 1-decanol, 4,5-octanedione, and δ-decalactone in step (3) and the GS prepared V6 The volume ratio of starch milk was 0.08-0.10:1, and the aqueous solution of 2-acetylpyridine and the prepared GS V7 The volume ratio of starch milk was 0.08-0.12:1, and the aqueous solution of α-pinene and the prepared GS V8 2. The method of claim 1, wherein the volume ratio of starch to milk is 0.10-0.12:
1.
5. The variable frequency ultrasonic treatment in step (3) is performed using ultrasonic waves having frequencies of 20 to 40, 40 to 60, and 60 to 80 kHz for 20 to 30, 10 to 20, and 0 to 10 min, respectively, with an on-off interval of 10 to 30 s. The method according to claim 1.
6. In step (2), different volume ratios of anhydrous alcohol and starch milk can be used to obtain classified starches with different degrees of polymerization, so only one volume ratio can be selected; Since different flavor molecule aqueous solutions can be used in step (3) to obtain different composite milks, only one type of composite milk is selected for cooling and crystallization. When an aqueous solution of 1-decanol, 4,5-octanedione or δ-decalactone is used, GS V6 When starch-complex milk is obtained and later cooled and crystallized, V 6I -, V 6II -, V 6III When an aqueous solution of 2-acetylpyridine is used, GS V7 When starch-complex milk is obtained and later cooled and crystallized, V 7 When an aqueous solution of α-pinene is used, GS V8 When starch-complex milk is obtained and later cooled and crystallized, V 8 -type crystalline starch is obtained, The method according to claim 1, wherein the aqueous solutions of 1-decanol, 4,5-octanedione, δ-decalactone, 2-acetylpyridine, and α-pinene are dispersions of various flavor substances, i.e., dispersions in which flavor substances are added to water and mixed uniformly.
7. Use of V-type crystalline starch complexed with flavour molecules according to the method of any one of claims 1 to 6 in the food sector.
8. A method for improving the embedding rate and flavor release effect of flavor molecules in starch-based foods, comprising: a step (1) of amorphization treatment, in which the high amylose starch is subjected to a dry heat amorphization treatment at 130-135°C for 10-12 minutes to obtain amorphized starch; Amorphous starch and water are prepared into a high-concentration starch milk of 30% to 40% by mass, and anhydrous ethanol is added to the starch milk so that the volume ratios of anhydrous ethanol to starch milk are 80% to 85%, 70% to 75%, and 55% to 60%, respectively. The mixture is then kept at 40 to 60°C for 30 to 40 minutes, and the alcohol precipitation product is separated to obtain GS having different polymerization degrees. V6 , G.S. V7 , G.S. V8 (2) a step of alcohol precipitation and classification to obtain a classified starch; Using plasma activated water, GS V6 , G.S. V7 , G.S. V8 The classified starches were each prepared into starch milk with a concentration of 5% to 7% by mass, and then aqueous solutions of 1-decanol, 4,5-octanedione, and δ-decalactone were added to the prepared GS. V6 GS was mixed with starch milk to prepare an aqueous solution of 2-acetylpyridine. V7 GS was mixed with starch milk to prepare an aqueous solution of α-pinene. V8 (3) a compounding step of mixing the starch milk with the starch milk to obtain a compound milk, sealing the compound milk, and subjecting the compound milk to variable frequency ultrasonic treatment to obtain a compound milk after variable frequency ultrasonic treatment; and (4) a cooling and crystallization step, in which the composite milk after the variable frequency ultrasonic treatment is rapidly cooled to 3-5°C at an average cooling rate of 5-10°C / min, crystallized at this temperature for 20-40 min, and then transferred to an environment of 20-30°C for crystallization for 2-4 h, followed by centrifuging, washing, drying and sieving to obtain a V-type crystalline starch complexed with flavor molecules.
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