Composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, oral product, and preparation method thereof

Abstract

The present invention discloses a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, an oral product, and a preparation method thereof. γ-Cyclodextrin, gum arabic, and part of resistant dextrin are dispersed in purified water, followed by addition of oyster oligopeptide powder, homogenization, low-temperature drying, and sizing to obtain pre-embedded oyster oligopeptide granules. The granules are post-mixed with black maca extract, L-citrulline, taurine, yeast zinc powder, and the remaining resistant dextrin, followed by dry granulation and sizing to obtain the composite premix. The composite premix has low water activity, low hygroscopicity, reduced oyster-derived fishy odor, good dispersibility and redispersibility in water, and improved macamide retention. The composite premix is suitable for preparing oral suspensions, hard capsules, and tablets for men's daily energy support, physical recovery, and nutritional supplementation.

Description

[0001] DESCRIPTION

[0002] Composite Premix Based on Ternary Pre-Embedding of Oyster Oligopeptide and Post-Mixing of Black Maca, Oral Product, and Preparation Method Thereof TECHNICAL FIELD

[0003] The present invention relates to the technical field of oral nutritional supplement products, and in particular relates to a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, an oral product, and a preparation method thereof.

[0004] BACKGROUND ART

[0005] Maca is a plant-derived raw material commonly used in men's daily nutritional supplement products. Oyster oligopeptide is a small-molecule peptide raw material prepared from oyster protein through processes such as enzymolysis, separation and drying. The combination of a maca raw material and oyster oligopeptide can be used in oral products for men's daily energy support, physical recovery and nutritional supplementation.

[0006] In the prior disclosed technologies, there have already existed solutions in which maca and oyster or oyster peptide are jointly used in oral products related to physical recovery, and there have also already existed solutions in which oyster oligopeptide is subjected to taste-masking embedding with materials such as cyclodextrin, maltodextrin, soy protein isolate or modified starch. Therefore, simply compounding maca with oyster oligopeptide, or simply subjecting oyster oligopeptide to conventional embedding for taste masking, makes it difficult to form a stable inventive basis.

[0007] Different from existing composite oral products that expand the formula scope by stacking a plurality of animal and plant nutritional raw materials, the present invention does not rely on increasing the number of formula components to form a technical contribution, but instead focuses on ternary pre-embedding of oyster oligopeptide, post-mixing of black maca extract and dry granulation, thereby improving low water activity, low fishy odor, low hygroscopicity, dispersibility in water and macamide stability of the composite premix.

[0008] Existing ordinary mixing, direct filling, direct tableting or ordinary wet granulation processes still have the following problems: oyster oligopeptide has an obvious marine fishy odor; both maca extract and oyster oligopeptide have certain hygroscopicity; macamide-type characteristic components in black maca extract haveDESCRIPTION

[0009] reduced stability under long-term water exposure and heat exposure; and when an ordinary mixed powder is used for an oral suspension, problems such as slow dispersion, agglomeration and difficulty in re-shaking uniformly after sedimentation easily occur. In view of this, a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, an oral product, and a preparation method thereof are proposed.

[0010] SUMMARY OF THE INVENTION

[0011] To solve the above technical problems, a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, an oral product, and a preparation method thereof are provided, and the present technical solution solves the above-described problems.

[0012] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, wherein the composite premix is prepared by post-mixing pre-embedded oyster oligopeptide granules with black maca extract, L-citrulline, taurine, yeast zinc powder and remaining resistant dextrin, and then subjecting the mixture to dry granulation;

[0013] wherein the pre-embedded oyster oligopeptide granules are prepared from oyster oligopeptide powder, y -cyclodextrin, gum arabic and part of the resistant dextrin through aqueous-phase dispersion, homogenization, low-temperature drying and sizing;

[0014] calculated in parts by weight on a dry basis after deducting moisture, the composite premix is composed, except for moisture, of the following components: 27.5-28.5 parts of black maca extract, 26.5-27.5 parts of oyster oligopeptide powder, 14.5-15.5 parts of L-citrulline, 7.8-8.2 parts of taurine, 4.8-5.2 parts of yeast zinc powder, 8.8-9.2 parts of y-cyclodextrin, 2.8-3.2 parts of gum arabic and 5.8-6.2 parts of resistant dextrin;

[0015] the moisture content of the composite premix is not higher than 5.0%, and the water activity is not higher than 0.45.

[0016] Preferably, the black maca extract is a black maca root extract, the extractionDESCRIPTION

[0017] ratio is 5:1, and the total macamide content is 0.20%-0.80%; the oyster oligopeptide powder has a protein content of not less than 65%, and peptide segments having a relative molecular weight of less than 1000 Da account for 70%-85% of the total peptide content of the oyster oligopeptide powder; and the yeast zinc powder has a zinc content of 8%- 12%.

[0018] Preferably, the mass ratio of the y-cyclodextrin, the gum arabic and the resistant dextrin is 8.8-9.2:2.8-3.2:5.8-6.2; wherein the resistant dextrin used for preparing the pre-embedded oyster oligopeptide granules accounts for 45%-55% of the total amount of resistant dextrin.

[0019] Preferably, the composite premix has a particle size of 20-60 mesh and an angle of repose of not higher than 35°.

[0020] An oral product based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, wherein the oral product is an oral suspension, a hard capsule or a tablet.

[0021] Preferably, each 20 mL of the oral suspension contains 0.8-1.2 g of the composite premix, 0.8-1.5 g of glycerol, 0.5-1.0 g of erythritol, 0.04-0.08 g of citric acid, 0.03-0.06 g of sodium citrate, 0.01-0.03 g of xanthan gum, 0.01-0.02 g of potassium sorbate, 0.01-0.04 g of food flavor and the balance of purified water, and has a pH of 4.2-4.8; after the oral suspension stands for 24 hours, a uniform suspension state can be re-formed by inverting it up and down 10 times.

[0022] Preferably, each hard capsule contains 450-550 mg of the composite premix, 2-6 mg of silicon dioxide and 2-6 mg of magnesium stearate; and each tablet contains 450-550 mg of the composite premix, 60-100 mg of microcrystalline cellulose, 90-140 mg of isomalt, 10-30 mg of croscarmellose sodium, 3-8 mg of silicon dioxide and 3-8 mg of magnesium stearate.

[0023] A method for preparing a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, wherein the preparation steps are as follows:

[0024] Step SI: adding y-cyclodextrin, gum arabic and part of the resistant dextrin toDESCRIPTION

[0025] purified water, and stirring at 38-44°C to obtain an embedding solution;

[0026] Step S2: adding oyster oligopeptide powder to the embedding solution obtained in Step SI, and subjecting the mixture to homogenization to obtain an oyster oligopeptide embedding wet material;

[0027] Step S3 : drying the oyster oligopeptide embedding wet material obtained in Step 52 at 45-52 ° C until the moisture content is not higher than 5.0%, and sizing the material to obtain pre-embedded oyster oligopeptide granules;

[0028] Step S4: mixing the pre-embedded oyster oligopeptide granules obtained in Step 53 with black maca extract, L-citrulline, taurine, yeast zinc powder and remaining resistant dextrin;

[0029] Step S5: subjecting the mixture obtained in Step S4 to dry granulation, and after sizing, obtaining the composite premix.

[0030] Preferably, in Step S2, the homogenization treatment has a rotational speed of 6000-7000 rpm and a homogenization time of 10-14 minutes.

[0031] Preferably, in Step S5, the dry granulation has a roll compaction pressure of 3.8-4.2 MPa, and the sizing screen is a 24-40 mesh screen.

[0032] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0033] The composite premix prepared by the present invention has characteristics of low water activity, low hygroscopicity, low oyster-derived fishy odor, good dispersibility in water and a high macamide retention rate, can be used for preparing oral suspensions, hard capsules and tablets, and is suitable as an oral product for men's daily energy support, physical recovery and nutritional supplementation; different from existing composite oral products that expand the formula scope by stacking a plurality of animal and plant nutritional raw materials, the present invention does not rely on increasing the number of formula components to form a technical contribution, but instead focuses on ternary pre-embedding of oyster oligopeptide, post-mixing of black maca extract and dry granulation, thereby improving low water activity, low fishy odor, low hygroscopicity, dispersibility inDESCRIPTION

[0034] water and macamide stability of the composite premix.

[0035] BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Fig. l is a flow chart of the preparation steps of the present invention.

[0037] DETAILED DESCRIPTION

[0038] The following description is provided to disclose the present invention so that those skilled in the art can practice the present invention. The preferred embodiments in the following description are merely examples, and those skilled in the art may conceive of other obvious variations.

[0039] Example 1 : Preparation of the Composite Premix

[0040] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0041] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder, 9.0 kg of y-cyclodextrin, 3.0 kg of gum arabic and 6.0 kg of resistant dextrin.

[0042] Raw material specifications:

[0043] Black maca extract: black maca root extract, extraction ratio 5:1, total macamide content 0.42%;

[0044] Oyster oligopeptide powder: protein content 72.4%, and peptide segments having a relative molecular weight of less than 1000 Da account for 78.1% of the total peptide content;

[0045] Yeast zinc powder: zinc content 10.0%.

[0046] Preparation steps:

[0047] Step SI: 9.0 kg of y-cyclodextrin, 3.0 kg of gum arabic and 3.0 kg of resistant dextrin (accounting for 50% of the total amount of resistant dextrin) were added to 36.0 kg of purified water, and stirred at 42°C for 25 minutes to obtain an embedding solution;

[0048] Step S2: 27.0 kg of oyster oligopeptide powder was slowly added to the embedding solution obtained in Step SI, and homogenized at a rotational speed of 6500 rpm for 12 minutes to obtain an oyster oligopeptide embedding wet material;

[0049] Step S3 : the oyster oligopeptide embedding wet material obtained in Step S2 wasDESCRIPTION

[0050] passed through a 20-mesh screen to prepare wet granules, dried in a fluidized bed at 48°C until the moisture content was not higher than 5.0%, and sized through a 30-mesh screen to obtain pre-embedded oyster oligopeptide granules;

[0051] Step S4: the pre-embedded oyster oligopeptide granules obtained in Step S3, 28.0 kg of black maca extract, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 3.0 kg of remaining resistant dextrin were put into a three-dimensional mixer and mixed for 25 minutes;

[0052] Step S5: the mixture obtained in Step S4 was subjected to dry granulation, with a roll compaction pressure of 4.0 MPa and a sizing screen of 30 mesh, to obtain a composite premix.

[0053] Product testing:

[0054] The resulting composite premix had a moisture content of 3.82%, a water activity of 0.38, a proportion of 20-60 mesh granules of 91.4%, and an angle of repose of31.8°.

[0055] Example 2: Preparation of the Composite Premix

[0056] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0057] 27.5 kg of black maca extract, 26.5 kg of oyster oligopeptide powder, 14.5 kg of L-citrulline, 7.8 kg of taurine, 4.8 kg of yeast zinc powder, 8.8 kg of y-cyclodextrin, 2.8 kg of gum arabic and 5.8 kg of resistant dextrin.

[0058] Raw material specifications:

[0059] Black maca extract: black maca root extract, extraction ratio 5:1, total macamide content 0.20%;

[0060] Oyster oligopeptide powder: protein content 65.0%, and peptide segments having a relative molecular weight of less than 1000 Da account for 70.0% of the total peptide content;

[0061] Yeast zinc powder: zinc content 8.0%.

[0062] Preparation steps:

[0063] Step SI: 8.8 kg of y-cyclodextrin, 2.8 kg of gum arabic and 2.6 kg of resistant dextrin (accounting for 45% of the total amount of resistant dextrin) were added toDESCRIPTION

[0064] 32.0 kg of purified water, and stirred at 38°C for 30 minutes to obtain an embedding solution;

[0065] Step S2: 26.5 kg of oyster oligopeptide powder was slowly added to the embedding solution obtained in Step SI, and homogenized at a rotational speed of 6000 rpm for 14 minutes to obtain an oyster oligopeptide embedding wet material;

[0066] Step S3 : the oyster oligopeptide embedding wet material obtained in Step S2 was passed through a 20-mesh screen to prepare wet granules, dried in a fluidized bed at 45°C until the moisture content was not higher than 5.0%, and sized through a 24-mesh screen to obtain pre-embedded oyster oligopeptide granules;

[0067] Step S4: the pre-embedded oyster oligopeptide granules obtained in Step S3, 27.5 kg of black maca extract, 14.5 kg of L-citrulline, 7.8 kg of taurine, 4.8 kg of yeast zinc powder and 3.2 kg of remaining resistant dextrin were put into a three-dimensional mixer and mixed for 30 minutes;

[0068] Step S5: the mixture obtained in Step S4 was subjected to dry granulation, with a roll compaction pressure of 3.8 MPa and a sizing screen of 24 mesh, to obtain a composite premix.

[0069] Product testing:

[0070] The resulting composite premix had a moisture content of 4.15%, a water activity of 0.41, a proportion of 20-60 mesh granules of 87.2%, and an angle of repose of33.5°.

[0071] Example 3 : Preparation of the Composite Premix

[0072] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0073] 28.5 kg of black maca extract, 27.5 kg of oyster oligopeptide powder, 15.5 kg of L-citrulline, 8.2 kg of taurine, 5.2 kg of yeast zinc powder, 9.2 kg of y-cyclodextrin, 3.2 kg of gum arabic and 6.2 kg of resistant dextrin.

[0074] Raw material specifications:

[0075] Black maca extract: black maca root extract, extraction ratio 5:1, total macamide content 0.80%;

[0076] Oyster oligopeptide powder: protein content 90.0%, and peptide segmentsDESCRIPTION

[0077] having a relative molecular weight of less than 1000 Da account for 85.0% of the total peptide content;

[0078] Yeast zinc powder: zinc content 12.0%.

[0079] Preparation steps:

[0080] Step SI: 9.2 kg of y-cyclodextrin, 3.2 kg of gum arabic and 3.4 kg of resistant dextrin (accounting for 55% of the total amount of resistant dextrin) were added to 40.0 kg of purified water, and stirred at 44°C for 20 minutes to obtain an embedding solution;

[0081] Step S2: 27.5 kg of oyster oligopeptide powder was slowly added to the embedding solution obtained in Step SI, and homogenized at a rotational speed of 7000 rpm for 10 minutes to obtain an oyster oligopeptide embedding wet material;

[0082] Step S3 : the oyster oligopeptide embedding wet material obtained in Step S2 was passed through a 20-mesh screen to prepare wet granules, dried in a fluidized bed at 52°C until the moisture content was not higher than 5.0%, and sized through a 40-mesh screen to obtain pre-embedded oyster oligopeptide granules;

[0083] Step S4: the pre-embedded oyster oligopeptide granules obtained in Step S3, 28.5 kg of black maca extract, 15.5 kg of L-citrulline, 8.2 kg of taurine, 5.2 kg of yeast zinc powder and 2.8 kg of remaining resistant dextrin were put into a three-dimensional mixer and mixed for 20 minutes;

[0084] Step S5: the mixture obtained in Step S4 was subjected to dry granulation, with a roll compaction pressure of 4.2 MPa and a sizing screen of 40 mesh, to obtain a composite premix.

[0085] Product testing:

[0086] The resulting composite premix had a moisture content of 3.56%, a water activity of 0.35, a proportion of 20-60 mesh granules of 93.8%, and an angle of repose of30.2°.

[0087] Example 4: Preparation of an Oral Suspension

[0088] Raw materials weighed out (calculated based on 1000 bottles, 20 mL per bottle):DESCRIPTION

[0089] 1000 g of the composite premix obtained in Example 1, 1200 g of glycerol, 800 g of erythritol, 60 g of citric acid, 50 g of sodium citrate, 20 g of xanthan gum, 4 g of sucralose, 15 g of potassium sorbate, 25 g of food-grade berry flavor and an appropriate amount of purified water.

[0090] Preparation steps:

[0091] (1) adding 20 g of xanthan gum to a portion of purified water (about 15 L), followed by stirring and swelling for 30 minutes;

[0092] (2) adding 1200 g of glycerol, 800 g of erythritol, 60 g of citric acid, 50 g of sodium citrate, 4 g of sucralose and 15 g of potassium sorbate to the swollen liquid obtained in step (1), followed by stirring to dissolve;

[0093] (3) adding 1000 g of the composite premix to the solution obtained in step (2), followed by high-speed shear dispersion for 8 minutes;

[0094] (4) adding 25 g of food-grade berry flavor to the suspension obtained in step (3), and supplementing purified water to a total volume of 20 L;

[0095] (5) degassing, filling and sealing the suspension obtained in step (4), holding it at 75°C for 15 minutes, and cooling to obtain the oral suspension.

[0096] Product testing:

[0097] The resulting oral suspension had a pH of 4.43, and after standing for 24 hours, a uniform suspension state could be re-formed by inverting it up and down 10 times.

[0098] Example 5: Preparation of Hard Capsules

[0099] Raw materials weighed out (calculated based on 1000 capsules):

[0100] 500 g of the composite premix obtained in Example 1, 4 g of silicon dioxide and 3 g of magnesium stearate.

[0101] Preparation steps:

[0102] (1) putting 500 g of the composite premix and 4 g of silicon dioxide into a three-dimensional mixer, followed by mixing for 12 minutes;

[0103] (2) adding 3 g of magnesium stearate to the mixture obtained in step (1), followed by further mixing for 3 minutes;

[0104] (3) filling the mixture obtained in step (2) into No. 0 HPMC hard capsules, withDESCRIPTION

[0105] a fill weight of about 507 mg per capsule.

[0106] Product testing:

[0107] Each resulting hard capsule contained about 500 mg of the composite premix, 4 mg of silicon dioxide and 3 mg of magnesium stearate. When 2 capsules were administered daily, the daily intake of the composite premix was about 1000 mg.

[0108] Example 6: Preparation of Tablets

[0109] Raw materials weighed out (calculated based on 1000 tablets):

[0110] 500 g of the composite premix obtained in Example 1, 80 g of microcrystalline cellulose, 120 g of isomalt, 20 g of croscarmellose sodium, 5 g of silicon dioxide and 5 g of magnesium stearate.

[0111] Preparation steps:

[0112] (1) putting 500 g of the composite premix, 80 g of microcrystalline cellulose, 120 g of isomalt, 20 g of croscarmellose sodium and 5 g of silicon dioxide into a three-dimensional mixer, followed by mixing for 20 minutes;

[0113] (2) adding 5 g of magnesium stearate to the mixture obtained in step (1), followed by further mixing for 3 minutes;

[0114] (3) tableting the mixture obtained in step (2) by using a rotary tablet press, and controlling the tablet weight to about 730 mg.

[0115] Product testing:

[0116] Each resulting tablet contained about 500 mg of the composite premix, 80 mg of microcrystalline cellulose, 120 mg of isomalt, 20 mg of croscarmellose sodium, 5 mg of silicon dioxide and 5 mg of magnesium stearate. The tablet hardness was 82 N, the friability was 0.39%, and the disintegration time limit was 18 min. When 2 tablets were administered daily, the daily intake of the composite premix was about 1000 mg.

[0117] Comparative Example 1 : Ordinary Mixed Powder

[0118] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0119] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 24.0 kg of microcrystalline cellulose (for making up the total weight).DESCRIPTION

[0120] Preparation steps:

[0121] All the above raw materials were put into a three-dimensional mixer and mixed for 30 minutes to obtain an ordinary mixed powder.

[0122] In Comparative Example 1, y-cyclodextrin, gum arabic and resistant dextrin were not added, pre-embedding treatment was not performed, and direct mixing was performed.

[0123] Comparative Example 2: P-Cyclodextrin Alone for Embedding

[0124] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0125] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 18.0 kg of P-cyclodextrin.

[0126] Preparation steps:

[0127] Step SI: 18.0 kg of P-cyclodextrin was added to 36.0 kg of purified water, and stirred at 42°C for 25 minutes to obtain an embedding solution;

[0128] Steps S2-S5: the same as in Example 1, except that the oyster oligopeptide powder was embedded only with single P-cyclodextrin.

[0129] Explanation: In Comparative Example 2, an equal amount of P-cyclodextrin was used to replace the ternary system of y-cyclodextrin, gum arabic and resistant dextrin.

[0130] Comparative Example 3 : y-Cyclodextrin Alone for Embedding

[0131] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0132] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 18.0 kg of y-cyclodextrin.

[0133] Preparation steps:

[0134] Step SI: 18.0 kg of y-cyclodextrin was added to 36.0 kg of purified water, and stirred at 42°C for 25 minutes to obtain an embedding solution;

[0135] Steps S2-S5: the same as in Example 1, except that the oyster oligopeptide powder was embedded only with single y-cyclodextrin.

[0136] In Comparative Example 3, an equal amount of y-cyclodextrin was used to

[0137] itDESCRIPTION

[0138] replace gum arabic and resistant dextrin, and only single y-cyclodextrin embedding was retained.

[0139] Comparative Example 4: Wet Granulation of All Raw Materials

[0140] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0141] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder, 9.0 kg of y-cyclodextrin, 3.0 kg of gum arabic and 6.0 kg of resistant dextrin.

[0142] Preparation steps:

[0143] (1) all the above raw materials were put into a mixer and mixed for 25 minutes; (2) purified water was added to the mixture until the moisture content was about 30%, thereby preparing wet granules;

[0144] (3) the wet granules were dried in a fluidized bed at 48°C until the moisture content was not higher than 5.0%;

[0145] (4) the granules were sized through a 30-mesh screen to obtain granules.

[0146] In Comparative Example 4, oyster oligopeptide was not separately pre-embedded, but all raw materials were mixed and then subjected to water-added wet granulation.

[0147] Comparative Example 5: Joint Wet Embedding of Black Maca Extract

[0148] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0149] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder, 9.0 kg of y-cyclodextrin, 3.0 kg of gum arabic and 6.0 kg of resistant dextrin.

[0150] Preparation steps:

[0151] Step SI: 9.0 kg of y-cyclodextrin, 3.0 kg of gum arabic and 3.0 kg of resistant dextrin were added to 36.0 kg of purified water, and stirred at 42°C for 25 minutes to obtain an embedding solution;

[0152] Step S2: 27.0 kg of oyster oligopeptide powder and 28.0 kg of black maca extract were simultaneously added to the embedding solution obtained in Step SI, and homogenized at a rotational speed of 6500 rpm for 12 minutes to obtain a mixed embedding wet material;DESCRIPTION

[0153] Step S3: the mixed embedding wet material obtained in Step S2 was passed through a 20-mesh screen to prepare wet granules, dried in a fluidized bed at 48°C until the moisture content was not higher than 5.0%, and sized through a 30-mesh screen to obtain pre-embedded granules;

[0154] Step S4: the pre-embedded granules obtained in Step S3, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 3.0 kg of remaining resistant dextrin were put into a three-dimensional mixer and mixed for 25 minutes;

[0155] Step S5: the mixture obtained in Step S4 was subjected to dry granulation, with a roll compaction pressure of 4.0 MPa and a sizing screen of 30 mesh, to obtain a composite premix.

[0156] In Comparative Example 5, the black maca extract and the oyster oligopeptide powder were added together to the embedding solution for wet embedding.

[0157] Comparative Example 6: Maltodextrin Replacing the Ternary System

[0158] Raw materials weighed out (calculated in parts by weight on a dry basis):

[0159] 28.0 kg of black maca extract, 27.0 kg of oyster oligopeptide powder, 15.0 kg of L-citrulline, 8.0 kg of taurine, 5.0 kg of yeast zinc powder and 18.0 kg of maltodextrin.

[0160] Preparation steps:

[0161] Step SI: 18.0 kg of maltodextrin was added to 36.0 kg of purified water, and stirred at 42°C for 25 minutes to obtain an embedding solution;

[0162] Steps S2-S5: the same as in Example 1, except that the oyster oligopeptide powder was embedded only with single maltodextrin.

[0163] In Comparative Example 6, an equal amount of maltodextrin was used to replace the ternary system of y-cyclodextrin, gum arabic and resistant dextrin.

[0164] Test Example 1 : Basic Physicochemical Properties

[0165] Detection methods:

[0166] Moisture: determined by a loss-on-drying method;

[0167] Water activity: determined by a water activity meter;

[0168] Particle size: determined by a standard sieve screening method for determiningDESCRIPTION

[0169] the proportion of 20-60 mesh granules;

[0170] Angle of repose: determined by a fixed funnel method.

[0171] The detection results are shown in Table 1 as basic physicochemical property detection results:

[0172] Sample Moisture / % Water activity Proportion of 20-60 Angle of repose / 0mesh / %

[0173] Example 1 3.82±0.09 0.38±0.01 91.4±1.6 31.8±0.7 Comparative 5.31±0.18 0.52±0.02 54.7±2.8 43.1±1.2 Example 1

[0174] Comparative 4.76±0.13 0.48±0.01 73.2±2.1 38.4±0.9 Example 2

[0175] Comparative 4.58±0.11 0.46±0.01 77.6±2.4 36.9±0.8 Example 3

[0176] Comparative 4.51±0.12 0.46±0.01 81.5±1.9 36.1±0.8 Example 4

[0177] Comparative 4.43±0.10 0.45±0.01 82.2±2.2 35.8±0.9 Example 5

[0178] Comparative 4.89±0.15 0.49±0.01 70.3±2.5 39.2±1.0 Example 6

[0179]

[0180] Table 1

[0181] The data in the table are expressed as mean ± standard deviation. Compared with Example 1, Comparative Example 1, Comparative Example 2 and Comparative Example 6 had statistically significant differences in moisture, water activity, proportion of 20-60 mesh granules and angle of repose (P < 0.05).

[0182] Result analysis:

[0183] Example 1 had statistically significant differences in moisture, water activity, proportion of 20-60 mesh granules and angle of repose as compared with Comparative Example 1, Comparative Example 2 and Comparative Example 6, indicating that the ternary pre-embedding system combined with the dry granulationDESCRIPTION

[0184] process of the present invention can effectively improve the physical properties of the product.

[0185] Test Example 2: Evaluation of Oyster-Derived Fishy Odor

[0186] Detection methods:

[0187] Twelve evaluators having received basic training were selected to conduct blind evaluation, and the samples were encoded with three-digit random codes. The scoring standard was 0-5 points, wherein 0 points indicated no obvious fishy odor, and 5 points indicated obvious and unacceptable fishy odor. Each sample of 5 g was added to 50 mL of warm water at 40°C, stirred for 30 seconds and then evaluated. Meanwhile, headspace injection-GC-MS was used to detect the relative response values of trimethylamine and dimethyl amine; the relative response value was a relative numerical value obtained by normalizing the peak area of the target volatile component with the peak area of an internal standard, and a lower value indicated fewer fishy-odor-related volatile components.

[0188] The detection results are shown in Table 2 as oyster-derived fishy odor evaluation results:

[0189] Sample Fishy odor score T ri methy lami nc relative Dimctlivlaminc relative response value response value Example 1 1.36±0.31 38.7±4.2 42.1±4.8 Comparative Example 1 3.84±0.52 119.5±9.8 126.3±10.5 Comparative Example 2 2.38±0.43 76.8±6.9 82.4±7.5 Comparative Example 3 2.16±0.39 69.2±6.1 74.5±6.8 Comparative Example 4 2.44±0.47 81.3±7.2 87.0±7.6 Comparative Example 5 2.31±0.44 75.9±6.5 80.7±6.9 Comparative Example 6 2.86±0.50 91.8±8.1 96.5±8.7

[0190]

[0191] Table 2

[0192] The data in the table are expressed as mean ± standard deviation. Compared with Example 1, the fishy odor scores and relative response values of volatile components of all comparative examples were higher, wherein Comparative Example 1,DESCRIPTION

[0193] Comparative Example 2 and Comparative Example 6 had statistically significant differences (P < 0.05).

[0194] Result analysis:

[0195] The fishy odor score, trimethylamine relative response value and dimethylamine relative response value of Example 1 were all lower than those of the comparative examples, and had statistically significant differences as compared with Comparative Example 1, Comparative Example 2 and Comparative Example 6. This indicates that the ternary pre-embedding system (y-cyclodextrin + gum arabic + resistant dextrin) of the present invention has a masking effect on the fishy odor of oyster oligopeptide superior to that of embedding with a single cyclodextrin or maltodextrin.

[0196] Test Example 3 : Hygroscopicity Test

[0197] Detection method:

[0198] Each sample of 10 g was spread flat in a weighing bottle and placed in a constant-temperature and constant-humidity chamber at 25°C and a relative humidity of 75%. The samples were weighed on day 1, day 3 and day 7, respectively, and the hygroscopic weight gain rate was calculated.

[0199] The detection results are shown in Table 3 as hygroscopicity test results:

[0200] Sample Day l / % Day 3 / % Day 7 / % Example 1 1.18±0.08 2.72±0.13 4.86±0.18 Comparative Example 1 3.42±0.21 7.36±0.34 11.25±0.46 Comparative Example 2 2.46±0.15 5.38±0.28 8.21±0.37 Comparative Example 3 2.21±0.13 4.97±0.25 7.62±0.31 Comparative Example 4 2.06±0.11 4.62±0.22 7.13±0.29 Comparative Example 5 2.02±0.12 4.55±0.24 6.91±0.28 Comparative Example 6 2.78±0.16 6.13±0.31 9.36±0.42

[0201]

[0202] Table 3

[0203] The data in the table are expressed as mean ± standard deviation. Compared with Example 1, the hygroscopic weight gain rates of all comparative examples on day 7 were higher, wherein Comparative Example 1, Comparative Example 2 andDESCRIPTION

[0204] Comparative Example 6 had statistically significant differences (P < 0.05).

[0205] Result analysis:

[0206] The hygroscopic weight gain rate of Example 1 on day 7 was lower than those of the comparative examples, and had statistically significant differences as compared with Comparative Example 1, Comparative Example 2 and Comparative Example 6. This indicates that the ternary pre-embedding system combined with the dry granulation process of the present invention can effectively reduce the hygroscopicity of the product.

[0207] Test Example 4: Dispersibility and Redispersibility in Water

[0208] Detection method:

[0209] A sample of 5 g was added to 100 mL of purified water at 25°C, stirred at 300 rpm, and the time required for basic dispersion without obvious large-particle agglomeration was recorded. After dispersion, the sample was allowed to stand for 24 hours, then inverted up and down 10 times, and the redispersion state was observed.

[0210] The redispersion score was evaluated on a scale of 1-5 points: 1 point indicated difficulty in redispersion, and 5 points indicated formation of a uniform suspension state after 10 inversions.

[0211] The detection results are shown in Table 4 as dispersibility and redispersibility in water test results:

[0212] Sample Initial dispersion timc / s Sedimentation state after standing Redispersion score after 10 for 24 h inversions Example 1 62±6 Slight sedimentation, no hard 4.8±0.2

[0213] caking

[0214] Comparative 226±18 Obvious agglomeration, hard 1.6±0.4 Example 1 bottom caking

[0215] Comparative 134±11 Relatively obvious sedimentation 3.1±0.3 Example 2

[0216] Comparative 118±10 Relatively obvious sedimentation 3.4±0.3 Example 3

[0217]

[0218] DESCRIPTION

[0219] Comparative 96±8 A small amount of fine 3.7±0.3 Example 4 agglomerates

[0220] Comparative 103±9 A small amount of fine 3.6±0.3 Example 5 agglomerates

[0221] Comparative 151±13 Obvious sedimentation 2.8±0.4 Example 6

[0222]

[0223] Table 4

[0224] The data in the table are expressed as mean ± standard deviation. Compared with Example 1, all comparative examples showed prolonged initial dispersion time and reduced redispersion scores, wherein Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 6 had statistically significant differences (P < 0.05).

[0225] Result analysis:

[0226] The initial dispersion time of Example 1 was shorter than those of the comparative examples, and the redispersion score was higher than those of the comparative examples, and had statistically significant differences as compared with Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 6. This indicates that the dry granulation process of the present invention can significantly improve dispersibility and redispersibility of the product in water.

[0227] Test Example 5: Macamide Stability

[0228] Detection method:

[0229] Each sample was sealed in an aluminum-plastic composite bag and placed in a constant-temperature and constant-humidity chamber at 40°C and a relative humidity of 75% for 3 months. The total macamide content was detected by HPLC, and the retention rate was calculated by taking the initial detection value as 100%.

[0230] The detection results are shown in Table 5 as macamide stability test results: Sample Initial total macamide content / mg gA-l Content after 3 months / mg gM Retention rate / %

[0231]

[0232] DESCRIPTION

[0233] Example 1 1.16±0.03 1.03±0.02 88.8±1.5 Comparative 1.15±0.03 0.88±0.02 76.5±1.9 Example 1

[0234] Comparative 1.14±0.03 0.89±0.02 78.1±1.7 Example 2

[0235] Comparative 1.15±0.03 0.92±0.02 80.0±1.6 Example 3

[0236] Comparative 0.98±0.03 0.71±0.02 72.4±2.1 Example 4

[0237] Comparative 0.95±0.03 0.67±0.02 70.5±2.2 Example 5

[0238] Comparative 1.14±0.03 0.89±0.02 78.1±1.8 Example 6

[0239]

[0240] Table 5

[0241] The data in the table are expressed as mean ± standard deviation. Compared with Example 1, Comparative Example 4 and Comparative Example 5 had reduced initial total macamide content and 3 -month retention rate; and the 3 -month retention rates of all comparative examples were lower than that of Example 1, with statistically significant differences (P < 0.05).

[0242] Result analysis:

[0243] Example 1 was superior to Comparative Example 4 and Comparative Example 5 in terms of the initial total macamide content and 3 -month retention rate; the 3 -month retention rate of Example 1 was higher than those of Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 6, with statistically significant differences.

[0244] The results show that, by using a process in which only the oyster oligopeptide is pre-embedded, the black maca extract is post-mixed and dry granulation is performed, Example 1 can reduce the water exposure and heat exposure of the black maca extract, thereby improving the retention level of macamide-type characteristic componentsDESCRIPTION

[0245] after preparation and during accelerated storage. The results of Comparative Example 4 and Comparative Example 5 show that if all raw materials are subjected to wet granulation or the black maca extract is subjected to joint wet embedding, not only is the initial total macamide content reduced, but the retention rate after accelerated storage for 3 months is further reduced.

[0246] Test Example 6: Observation of Adaptability to Different Dosage Forms Detection method:

[0247] The oral suspension of Example 2, the hard capsules of Example 3 and the tablets of Example 4 were placed at 40°C for 30 days, and the appearance, odor and key quality indicators were observed.

[0248] The detection results are shown in Table 6 as observation results of adaptability to different dosage forms:

[0249] Sample Appearance Odor Kc\ quality indicator Change after 30 days Oral suspension Brownish-yellow to No obvious return of pH 4.43; slight Uniformity restored dark brown fishy odor sedimentation after shaking suspension

[0250] Hard capsule Capsules intact, No obvious return of Moisture content of No obvious caking contents loose fishy odor contents 4.05%

[0251] Tablet Tablet surface intact, No obvious return of Hardness 82 N, No obvious change no cracking fishy odor friability 0.39%, in indicators disintegration 18

[0252] min

[0253]

[0254] Table 6

[0255] The results in the table are observation results after standing at 40°C for 30 days, and are used to illustrate the dosage-form adaptability of the composite premix in oral suspensions, hard capsules and tablets.

[0256] The above examples and test examples show that the present invention adopts a ternary system of y-cyclodextrin, gum arabic and resistant dextrin to pre-embed oyster oligopeptide, post-mixes black maca extract and then performs dry granulation,DESCRIPTION

[0257] thereby effectively improving fishy odor, hygroscopicity, dispersibility in water and macamide stability of the composite premix. Compared with the comparative examples, the present invention has significant advantages in all performance indicators. The resulting composite premix can be further prepared into oral suspensions, hard capsules and tablets, and is suitable as an oral product for men's daily energy support, physical recovery and nutritional supplementation.

[0258] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and what is described in the above embodiments and the description is only the principle of the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention, and these changes and improvements all fall within the scope of the claimed invention.

Claims

CLAIMS1. A composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, characterized in that: the composite premix is prepared by post-mixing pre-embedded oyster oligopeptide granules with black maca extract, L-citrulline, taurine, yeast zinc powder and remaining resistant dextrin, and then subjecting the resulting mixture to dry granulation;wherein the pre-embedded oyster oligopeptide granules are prepared from oyster oligopeptide powder, y -cyclodextrin, gum arabic and part of the resistant dextrin through aqueous-phase dispersion, homogenization, low-temperature drying and sizing;calculated in parts by weight on a dry basis after deducting moisture, the composite premix is composed, except for moisture, of the following components: 27.5-28.5 parts of black maca extract, 26.5-27.5 parts of oyster oligopeptide powder, 14.5-15.5 parts of L-citrulline, 7.8-8.2 parts of taurine, 4.8-5.2 parts of yeast zinc powder, 8.8-9.2 parts of y-cyclodextrin, 2.8-3.2 parts of gum arabic and 5.8-6.2 parts of resistant dextrin;the moisture content of the composite premix is not higher than 5.0%, and the water activity is not higher than 0.45.

2. The composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 1, characterized in that: the black maca extract is a black maca root extract, the extraction ratio is 5:1, and the total macamide content is 0.20%-0.80%; the oyster oligopeptide powder has a protein content of not less than 65%, and peptide segments having a relative molecular weight of less than 1000 Da account for 70%-85% of the total peptide content of the oyster oligopeptide powder; and the yeast zinc powder has a zinc content of 8%-12%.

3. The composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 1, characterized in that: the mass ratio of the y-cyclodextrin, the gum arabic and the resistant dextrin is 8.8-9.2:2.8-3.2:5.8-6.2; wherein the resistant dextrin used for preparing the pre-embedded oyster oligopeptide granules accounts for 45%-55% of the total amountCLAIMSof resistant dextrin.

4. The composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 1, characterized in that: the composite premix has a particle size of 20-60 mesh and an angle of repose of not higher than 35°.

5. An oral product based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, applied to the composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to any one of claims 1 to 4, characterized in that: the oral product is an oral suspension, a hard capsule or a tablet.

6. The oral product based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 5, characterized in that: each 20 mL of the oral suspension contains 0.8-1.2 g of the composite premix, 0.8-1.5 g of glycerol, 0.5-1.0 g of erythritol, 0.04-0.08 g of citric acid, 0.03-0.06 g of sodium citrate, 0.01-0.03 g of xanthan gum, 0.01-0.02 g of potassium sorbate, 0.01-0.04 g of food flavor and the balance of purified water, and has a pH of 4.2-4.8; after the oral suspension stands for 24 hours, a uniform suspension state can be re-formed by inverting it up and down 10 times.

7. The oral product based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 5, characterized in that: each hard capsule contains 450-550 mg of the composite premix, 2-6 mg of silicon dioxide and 2-6 mg of magnesium stearate; and each tablet contains 450-550 mg of the composite premix, 60-100 mg of microcrystalline cellulose, 90-140 mg of isomalt, 10-30 mg of croscarmellose sodium, 3-8 mg of silicon dioxide and 3-8 mg of magnesium stearate.

8. A method for preparing a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca, applied to the composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to any one of claims 1 to 4, characterized in that the preparation steps are as follows:CLAIMSStep SI: adding y-cyclodextrin, gum arabic and part of the resistant dextrin to purified water, and stirring at 38-44°C to obtain an embedding solution;Step S2: adding oyster oligopeptide powder to the embedding solution obtained in Step SI, and subjecting the mixture to homogenization to obtain an oyster oligopeptide embedding wet material;Step S3 : drying the oyster oligopeptide embedding wet material obtained in Step 52 at 45-52°C until the moisture content is not higher than 5.0%, and sizing the material to obtain pre-embedded oyster oligopeptide granules;Step S4: mixing the pre-embedded oyster oligopeptide granules obtained in Step 53 with black maca extract, L-citrulline, taurine, yeast zinc powder and remaining resistant dextrin;Step S5: subjecting the mixture obtained in Step S4 to dry granulation, and after sizing, obtaining the composite premix.

9. The method for preparing a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 8, characterized in that: in Step S2, the homogenization treatment has a rotational speed of 6000-7000 rpm and a homogenization time of 10-14 minutes.

10. The method for preparing a composite premix based on ternary pre-embedding of oyster oligopeptide and post-mixing of black maca according to claim 8, characterized in that: in Step S5, the dry granulation has a roll compaction pressure of 3.8-4.2 MPa, and the sizing screen is a 24-40 mesh screen.

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