Improved method

Abstract

The present invention relates to an improved process, in particular to a novel process for the preparation of a more stable formulation of Vitamin C (or Vitamin C derivative).

Description

[0001] This application is a divisional application of Chinese patent application No. 201880009695.6 (PCT / EP2018 / 052393) entitled "Improved Method", filed by the applicant DSM Intellectual Property Asset Management Co., Ltd. on January 31, 2018. Technical Field

[0002] This invention relates to a novel method for preparing a more stable vitamin C (or vitamin C derivative) formulation. Background Technology

[0003] Vitamin C is essential for farmed fish and shrimp. Fish and shrimp cannot synthesize vitamin C themselves, so they must obtain it through their diet.

[0004] Vitamin C is required for the following: • Growth and development • Reproduction • Wound healing • Disease resistance and the immune capacity of the immune system.

[0005] Vitamin C also has some issues with its stability, so it needs to be protected.

[0006] In aquaculture, it is also common to use vitamin C derivatives instead of vitamin C. One very common and widely used vitamin C derivative is L-ascorbic acid-2-monophosphate.

[0007] L-Ascorbic acid-2-monophosphate is a more stable derivative form of vitamin C, which has excellent properties and is now used in many fish and shrimp farms.

[0008] This vitamin C derivative is L-ascorbic acid-2-monophosphate, which is represented by the following formula (I).

[0009] Such vitamin C derivatives are, for example, marketed under the brand name ROVIMIX. ® STAY-C ® 35 and STAY-C ® 50 were purchased from DSM.

[0010] In some applications, L-ascorbic acid-2-monophosphate is added to a feed form and subsequently coated with oil before being fed to fish or shrimp. A drawback of this type of application is that some vitamin C (or its derivatives) is lost when the form is soaked in water for an extended period. Summary of the Invention

[0011] This invention provides a method for preparing a vitamin-rich aquatic feed composition, the method comprising: • Forms an aqueous solution containing a vitamin C source and a buffer; • The gel polymer is dispersed into the aqueous solution under stirring conditions to obtain a homogeneous mixture; • Introducing a divalent cation source into the mixture to induce gel formation, thereby preparing a vitamin-containing gel; • The gel is dried to obtain a dry gel powder encapsulated with a vitamin C source; • Dry gel powder is rehydrated in water in the presence of one or more viscosity-modified polysaccharides to form a stable suspension; • The suspension is brought into contact with an aquatic feed composition (such as shrimp feed), allowing the suspension to be adsorbed onto or incorporated into the feed matrix to obtain a fortified feed composition; and • The retention of vitamins in fortified feed compositions is assessed by immersing the feed in an aqueous medium, and the release of vitamins in the medium over time is determined. Attached Figure Description

[0012] Figure 1 The retention rates of Stay-C in feed pellets at the end of immersion in water for 10 min, 30 min, and 60 min are shown. Detailed Implementation

[0013] Therefore, the object of this invention is to find a way to make the formulation more stable using an easy-to-implement method.

[0014] Surprisingly, it was found that a more stable feed form was obtained when vitamin C (or its derivatives) was mixed with at least one gum and subsequently suspended in water before being added to the feed. Furthermore, this method can be performed with minimal technical equipment. In fact, it can be done with kitchen appliances or even without any electrical equipment at all.

[0015] Therefore, the present invention relates to a method (P) for preparing a feed formulation, the method comprising the following steps: (i) A gel is formed by adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin gelatin, and modified cellulose (such as methylcellulose, ethylcellulose, etc.), and gelling the mixture. (ii) Mix the gel from step (i) with (commercially available) fish or shrimp feed.

[0016] The resulting formulation is more stable in terms of vitamin C (and / or vitamin C derivatives) loss when immersed in water.

[0017] This is a very important advantage for fish or shrimp farmers.

[0018] Because of the simplicity of this method, simple household (kitchen) appliances (such as electric mixers) or just a whisk can be used.

[0019] Clearly, this method can also be performed using industrial equipment.

[0020] The improved formulation thus obtained is a feed formulation for fish and / or shrimp. Therefore, all ingredients and their amounts used in the method according to the invention are those ingredients and their amounts approved for use in such feed formulations.

[0021] The steps of the method are discussed in further detail.

[0022] Step (i): Vitamin C and / or at least one vitamin C derivative are added to the gel-forming compound and gel the mixture ) The first step was completed using existing technology.

[0023] Typical gel-forming compounds include natural gums, starch, pectin, gellan gum, agar-agar, and gelatin. They are usually based on polysaccharides or proteins.

[0024] Suitable gel-forming compounds include, for example: Alginate, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin, gelatin, and modified cellulose (such as methylcellulose, ethylcellulose, etc.).

[0025] Therefore, the present invention relates to a method (P1) that is a method (P) wherein the at least one gel-forming compound in step (i) is selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin gelatin and modified cellulose (such as methylcellulose, ethylcellulose, etc.).

[0026] The gelation process of gelling agents can be initiated as is well known. Typically, gelation is initiated by cations (such as Ca²⁺, ... 2+ Mg 2+ Na + and K + Initiated by the addition of the cation as an aqueous solution of a salt (such as CaCl2, MgCl2, NaCl, and KCl) to the gel-forming compound.

[0027] Typically and preferably, vitamin C and / or vitamin C derivatives are added to water, followed by the addition of a gel-forming compound, and finally a gelation process is carried out. Alternatively, a solution of vitamin C and / or vitamin C derivatives can be added to the gel-forming compound.

[0028] In cases where vitamin C derivatives are not very water-soluble (such as L-ascorbic acid-2-monophosphate), the vitamin C derivative must be converted into a water-soluble form.

[0029] For example, converting L-ascorbic acid-2-monophosphate into a water-soluble salt.

[0030] Step (i) is typically performed at ambient temperature. Heating the mixture is not required.

[0031] Step (ii): Mix the gel from step (i) with (commercially available) fish or shrimp feed. ) In this step, the gel obtained from step (i) is added to the feed formulation. The feed can be any type of feed (or commercially available feed) that is fortified with vitamin C and / or vitamin C derivatives (or the feed is added to vitamin C and / or vitamin C derivatives).

[0032] Mix under stirring (mechanical or manual stirring).

[0033] The fortified feed formulation thus obtained can be used as is, or further fortified and / or used in any other suitable application if needed.

[0034] Furthermore, it is possible that the method according to the invention may have additional steps. The formulation may also be dried after gelation. This can be advantageous when the method is not carried out in a single location and / or at the same point in time. The spray-dried form can be stored, and this form is storage stable.

[0035] Therefore, the present invention relates to a method for preparing a feed formulation (P2), the method comprising the following steps: a. Adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin gelatin, and modified cellulose (such as methylcellulose, ethylcellulose, etc.), and gelling. b. Spray-dry the gel form from step a. c. Mix the spray-dried form from step b with at least one adhesive, and suspend the mixture in water. d. Mix the suspended solids from step c with (commercially available) fish or shrimp feed.

[0036] Therefore, the present invention relates to a method for preparing a feed formulation (P3), which comprises the following steps: a. Adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin gelatin, and modified cellulose (such as methylcellulose, ethylcellulose, etc.), and gelling. b. Spray-dry the gel form from step a. c. Mix the spray-dried form from step b with at least one adhesive, and suspend the mixture in water. d. Mix the suspended solids from step c with (commercially available) fish or shrimp feed.

[0037] Steps (a) and (c) are similar to steps (i) and (ii) of methods (P) and (P1).

[0038] The four steps (especially the two additional steps) are discussed in more detail.

[0039] Step (a): Adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming agent In the compound and gelation. ) The first step was completed using existing technology.

[0040] Typical gel-forming compounds include natural gums, starch, pectin, gellan gum, agar-agar, and gelatin. They are usually based on polysaccharides or proteins.

[0041] Suitable gel-forming compounds include, for example: Alginate, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, gellan gum, carrageenan, locust bean gum, pectin, gelatin, and modified cellulose (such as methylcellulose, ethylcellulose, etc.).

[0042] The gelation process of gelling agents can be initiated as is well known. Typically, gelation is initiated by cations (such as Ca²⁺, ... 2+ Mg 2+ Na + and K + Initiated by the addition of the cation as an aqueous solution of a salt (such as CaCl2, MgCl2, NaCl, and KCl) to the gel-forming compound.

[0043] Typically and preferably, vitamin C and / or vitamin C derivatives are added to water, followed by the addition of a gel-forming compound, and finally a gelation process is carried out. Alternatively, a solution of vitamin C and / or vitamin C derivatives can be added to the gel-forming compound.

[0044] In cases where vitamin C derivatives are not very water-soluble (such as L-ascorbic acid-2-monophosphate), the vitamin C derivative must be converted into a water-soluble form.

[0045] For example, converting L-ascorbic acid-2-monophosphate into a water-soluble salt.

[0046] Step (a) is typically performed at ambient temperature. Heating the mixture is not required. The amount of vitamin C and / or vitamin C derivatives contained in the gel can be adjusted according to the solubility of vitamin C and / or vitamin C derivatives.

[0047] Step (b): Spray dry the gel form from step a. ) Now, the gel obtained from step (a) can be spray-dried using commonly known spray drying methods.

[0048] A very suitable spray drying method is to use a benchtop spray dryer (with an inlet temperature of approximately 120°C-170°C and an outlet temperature of 50-90°C).

[0049] The products obtained in this way can be stored as needed.

[0050] Step (c): The spray-dried form of step b is mixed with at least one adhesive, and the mixture is... The object is suspended in the water ) The spray-dried product obtained in step b is suspended in water, and typically and preferably, at least one gumming agent is added to the suspension. This gumming agent can be natural or synthetic. Suitable gumming agents are, for example, guar gum, xanthan gum, modified starch, and carboxymethyl cellulose, as well as hydroxyethyl cellulose.

[0051] Suspended solids are usually generated during agitation.

[0052] Step (c) is typically performed at ambient temperature. Heating the mixture is not required.

[0053] The ratio of the spray-dried product obtained from step b to the gelling agent added in step c can be adjusted according to the target concentration of vitamin C and / or vitamin derivatives in the fish / shrimp feed.

[0054] Step (d): Mix the suspended solids from step c with (commercially available) fish or shrimp feed. ) In this step, the suspension obtained from step (c) is added to the feed formulation. The feed can be any type of feed (or commercially available feed) that is fortified with vitamin C and / or vitamin C derivatives (or the feed is added to vitamin C and / or vitamin C derivatives).

[0055] Mix under stirring (mechanical or manual stirring).

[0056] The fortified feed formulation thus obtained can be used as is, or further fortified and / or used in any other suitable application if needed.

[0057] The following examples further illustrate the invention, but are not intended to limit it. Unless otherwise stated, all percentages and parts given are by weight, and temperatures are given in °C.

[0058] Figure 1 The retention rate of Stay-C in feed pellets at the end of immersion in water for 10 min, 30 min, and 60 min. This application includes the following implementation methods: Implementation Method 1. A method for preparing a feed formulation, the method comprising the following steps: (i) A gel is formed by adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, carrageenan, locust bean gum, pectin gelatin, and modified cellulose, and (ii) Mix the gel from step (i) with (commercially available) fish or shrimp feed.

[0059] Implementation Method 2. The method according to Implementation Method 1, wherein the steps of the method are performed using a household kitchen appliance.

[0060] Implementation Method 3. The method according to any one of the foregoing embodiments, wherein the vitamin C derivative is L-ascorbic acid-2-monophosphate.

[0061] Implementation Method 4. The method according to any one of the foregoing embodiments, wherein the mixing in step (ii) is carried out under stirring (mechanical stirring or manual stirring).

[0062] Implementation Method 5. The method according to any one of the foregoing embodiments, wherein the method has additional steps.

[0063] Implementation Method 6. The method according to Implementation Method 5, wherein the method includes the following steps: a. Adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, carrageenan, locust bean gum, pectin gelatin, and modified cellulose, and gelling the mixture, and then performing gelation. b. Spray-dry the gel form obtained in step a, and c. The spray-dried form of step b is mixed with at least one adhesive, and the mixture is suspended in water. d. Mix the suspended matter from step c with (commercially available) fish or shrimp feed.

[0064] Implementation Method 7. The method according to Implementation Method 5, wherein the method comprises the following steps: a. Adding vitamin C and / or at least one vitamin C derivative to at least one gel-forming compound selected from the group consisting of: alginic acid, sodium alginate, potassium alginate, ammonium alginate, calcium alginate agar, carrageenan, locust bean gum, pectin gelatin, and modified cellulose, and gelling the mixture, and then performing gelation. b. Spray-dry the gel form obtained in step a, and c. The spray-dried form of step b is mixed with at least one adhesive, and the mixture is suspended in water. d. Mix the suspended matter from step c with (commercially available) fish or shrimp feed.

[0065] Implementation Method 8. The method according to Implementation Method 6 or 7, wherein the vitamin C derivative is L-ascorbic acid-2-monophosphate.

[0066] Implementation 9. The method according to any one of Implementations 6 to 8, wherein the spray drying in step (b) is performed by a benchtop spray dryer.

[0067] Embodiment 10. The method according to any one of Embodiments 7 to 9, wherein the adhesive in step (d) is selected from the group consisting of guar gum, xanthan gum, modified starch, and carboxymethyl cellulose and hydroxyethyl cellulose.

[0068] Implementation Method 11. The method according to any one of Implementation Methods 7 to 10, wherein the suspension in step (c) is generated under stirring.

[0069] Example Example 1: In a glass beaker, add 0.1 g sodium citrate and 10 g Stay-C ® Dissolve (purchased from DSM) in 75 g of deionized water and mix. Then slowly add 0.08 g of low-acyl gellan gum to the water and mix continuously for 30 min.

[0070] Then, 15 g of 2% CaCl2 aqueous solution was added dropwise to the solution to initiate gel formation, and the mixture was continuously mixed for 15 min.

[0071] The prepared gel solution was then pumped under mixed conditions into a benchtop spray dryer with an inlet temperature of 150°C and an outlet temperature of 66°C. The spray-dried gel powder was collected and stored.

[0072] Then 10 g of the spray-dried Stay-C ® Gel powder, 0.7 g guar gum powder and 0.3 g xanthan gum powder were added together to 89 g deionized water and mixed at 600 rpm for 20-30 min to obtain a uniform suspension.

[0073] Finally, the suspension prepared by 25 g of commercially available shrimp feed and 0.5 g (20 g / kg feed) was mixed in a round-bottom flask by manual shaking, and then rotated in a rotary evaporator for 15-30 min to absorb the residual suspension on the flask.

[0074] The vitamin C stability of the fortified feed formulation thus obtained was then tested.

[0075] For this purpose, an immersion test was conducted.

[0076] For the immersion test, the test feed (in this embodiment of the invention) and the control feed were immersed in 1500g of deionized water in a glass beaker and kept still throughout the immersion test. The L-ascorbic acid-2-monophosphate level in the water was analyzed at 10 min, 30 min, and 60 min. The feed pellets were weighed and the dry matter content was analyzed. The retention percentage was then calculated.

[0077] The control diet was produced as follows: 10 g Stay-C ® Dissolve in 90 g of deionized water. Then spray 0.5 g of the solution onto 25 g of commercially available feed. StayC ® The levels were the same as those in the test feed.

[0078] Test results are summarized in Figure 1 In this study, it can be seen that the feed formulation produced by the method according to the present invention exhibits significantly improved stability.

Claims

1. A method for preparing a vitamin-rich aquatic feed composition, the method comprising: • Forms an aqueous solution containing a vitamin C source and a buffer; • The gel polymer is dispersed into the aqueous solution under stirring conditions to obtain a homogeneous mixture; • Introducing a divalent cation source into the mixture to induce gel formation, thereby preparing a vitamin-containing gel; • The gel is dried to obtain a dry gel powder encapsulated with a vitamin C source; • Dry gel powder is rehydrated in water in the presence of one or more viscosity-modified polysaccharides to form a stable suspension; • Contact the suspension with an aquatic feed composition (such as shrimp feed) so that the suspension is adsorbed onto or into the feed matrix to obtain a fortified feed composition. and • The retention of vitamins in fortified feed compositions is assessed by immersing the feed in an aqueous medium, and the release of vitamins in the medium over time is determined.

2. The method according to claim 1, wherein the method is performed using a household kitchen appliance.

3. The method according to any one of claims 1 to 2, wherein the drying is performed by a benchtop spray dryer.

4. The method according to any one of claims 1 to 3, wherein the suspension is generated under stirring.

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