A kind of flavor-retaining flavoring oil microcapsule powder and its preparation method and application

Abstract

The present invention provides a flavor-retaining flavor oil microcapsule powder and a preparation method and application thereof. The flavor-retaining flavor oil microcapsule powder is made of NLC emulsion and wall material, wherein the NLC emulsion contains a core material and an aqueous phase in a mass ratio of 1 to 3:7 to 9; the mass ratio of the core material to the wall material is 1:1 to 6; the core material contains a solid fat and flavor oil in a mass ratio of 1 to 36:4, and the solid fat is a solid fat with a melting point above 35°C. In the above-mentioned flavor-retaining flavor oil microcapsule powder, the solid fat and the wall material not only synergistically improve the water solubility of the flavor oil, reduce the volatilization of the flavor oil, and enhance the embedding rate, oxidative stability and fluidity of the flavor oil; more importantly, they show significant synergistic effects in the retention and release of aroma components, achieving long-term retention of the aroma components and their controllable release.

Description

Technical Field

[0001] The present invention belongs to the field of microcapsule technology, and more specifically, relates to a flavor-retaining flavoring oil microcapsule powder, and a preparation method and application thereof. Background Art

[0002] Seasoning oils can bring a pleasant taste to diners because of their characteristic flavor substances. For example, mustard oil, as the main aroma component of mustard, can stimulate the secretion of saliva and gastric juice, and has the effect of whetting and enhancing appetite; another example is prickly ash oleoresin, as the main aroma component of prickly ash, which can bring a spicy taste to diners. Seasoning oils all have very strong aroma components, but seasoning oils themselves have poor stability and are very sensitive to light, heat and oxygen. They are easy to evaporate in a short time, and their aroma components have a short retention time and are easy to lose. This results in the characteristic taste and aroma of seasoning oils often being lost during the shelf life of processed foods, greatly affecting the flavor and taste of processed foods, and seriously limiting the promotion and application of processed foods.

[0003] At present, in order to improve the stability of seasoning oil, seasoning oil is often made into an emulsion, then wrapped with a polymer material, and finally made into a microcapsule product through spray drying, so that the seasoning oil can be isolated from the external environment and reduce the contact of the seasoning oil with light, heat and oxygen. However, the stability of the seasoning oil in the microcapsule product obtained in this way is still relatively limited, and the controllability of aroma release cannot be achieved. There are still defects such as short retention time and easy loss of aroma components. Summary of the invention

[0004] The present invention aims to provide a flavor-retaining flavor oil microcapsule powder, which can improve the stability of the flavor oil and achieve long-term retention and controllable release of the flavor components.

[0005] The first object of the present invention is to provide a flavor-retaining flavoring oil microcapsule powder.

[0006] The second object of the present invention is to provide a method for preparing the above-mentioned flavor-retaining flavor oil microcapsule powder.

[0007] The third object of the present invention is to provide the use of the above-mentioned flavor-retaining flavoring oil microcapsule powder in the preparation of processed foods.

[0008] The above-mentioned purpose of the present invention is achieved through the following technical solutions:

[0009] The invention provides a flavor-retaining flavoring oil microcapsule powder, which is made of an NLC emulsion and a wall material, wherein the NLC emulsion comprises a core material and an aqueous phase in a mass ratio of 1-3:7-9; the mass ratio of the core material to the wall material is 1:1-6; the core material comprises a solid fat and flavoring oil in a mass ratio of 1-36:4, and the solid fat is a solid fat with a melting point above 35°C.

[0010] The present invention uses solid fat that is solid at room temperature to replace part of the seasoning oil in the core material, emulsifies to obtain a nanostructured lipid carrier (NLC) emulsion, and then combines it with a wall material to form a microcapsule powder. Compared with microcapsules made of traditional nanoemulsions, the present invention has the following obvious advantages: 1) The addition of solid fat increases the steric hindrance between droplets, significantly improves the storage stability at room temperature, and is not prone to unstable phenomena such as phase stratification, droplet flocculation, polymerization, and Austenosis; 2) Solid fat and wall material synergistically improve the water solubility of seasoning oil, reduce the volatilization of seasoning oil, and improve the embedding rate, oxidative stability and fluidity of seasoning oil; 3) Solid fat and wall material show significant synergistic effects in the retention and release of aroma components, achieving long-term retention of aroma components and their controllable release.

[0011] Preferably, the aqueous phase comprises an emulsifier and water, and the concentration of the emulsifier in the aqueous phase is 1-4% (w / w).

[0012] Preferably, the seasoning oil comprises one or more of mustard oil, sesame oil, Sichuan pepper oil, Sichuan pepper oil, and chili oil.

[0013] Preferably, the solid fat comprises one or more of cocoa butter (melting point is 38° C.), beeswax (melting point is 67° C.), animal fat, and stearic acid (melting point is 72° C.).

[0014] Further preferably, the animal fat includes but is not limited to beef tallow (melting point is 46° C.).

[0015] Preferably, the wall material is a protein wall material and / or a carbohydrate wall material.

[0016] More preferably, the protein wall material is one or more of soy protein isolate, casein, and whey protein isolate.

[0017] More preferably, the carbohydrate wall material is one or more of maltodextrin, modified starch, vegetable gum, and β-cyclodextrin.

[0018] More preferably, the vegetable gum is gum arabic.

[0019] Preferably, the emulsifier is a hydrophilic emulsifier or an amphiphilic emulsifier.

[0020] More preferably, the hydrophilic emulsifier is one or more of Tween 20, Tween 80, and sucrose laurate.

[0021] More preferably, the amphiphilic emulsifier is one or more of Span 20, soy lecithin, and sodium caseinate.

[0022] The present invention also provides a method for preparing the above-mentioned flavor-retaining flavoring oil microcapsule powder, which specifically comprises the following steps:

[0023] S1. The solid fat is heated until completely melted, and then mixed with the seasoning oil to obtain a core material;

[0024] S2. dissolving the emulsifier in water to obtain an aqueous phase;

[0025] S3. Hydrate the wall material until it is completely dissolved to obtain a wall material solution;

[0026] S4. The core material obtained in S1 and the aqueous phase obtained in S2 are mixed and sheared, homogenized or ultrasonicated, and then cooled to obtain an NLC emulsion;

[0027] S5. The wall material solution obtained in S3 and the NLC emulsion obtained in S4 were mixed and spray-dried to obtain the flavor-retaining flavoring oil microcapsule powder;

[0028] The mixing temperature in S4 needs to be at least 5° C. higher than the melting point of the solid fat; and the execution order of S1, S2, and S3 is not limited.

[0029] The term “S1, S2, S3 are not limited in execution order” means that S1 may be executed first, S2 may be executed first, S3 may be executed first, or they may be executed simultaneously.

[0030] Preferably, before the mixing in S4, the temperature of the core material and the water phase are both higher than the melting point of the solid fat by more than 5°C, such as 5-10°C higher.

[0031] Further preferably, the temperature of the heating in S1 and the dissolving in S2 are both higher than the melting point of the solid fat by more than 5° C., such as 5-10° C. higher.

[0032] Preferably, the shearing temperature in S4 is higher than the melting point of the solid fat by more than 5°C, such as 5-10°C higher.

[0033] Preferably, the shearing in S4 is shearing at 8000-15000 rpm for 2-10 min.

[0034] Preferably, the homogenization temperature in S4 is higher than the melting point of the solid fat by more than 5° C., such as 5-10° C. higher.

[0035] Preferably, the homogenization in S4 is carried out at 500-1000 bar for 3-7 times.

[0036] Preferably, the temperature of the ultrasound in S4 is at least 5°C higher than the melting point of the solid fat, such as 5-10°C higher.

[0037] Preferably, the ultrasound in S4 is performed at 100-500W for 4-15min.

[0038] Preferably, the cooling in S4 is cooling at -20 to 25°C.

[0039] Preferably, the cooling time in S4 is 20 to 40 minutes.

[0040] Preferably, the mixing in S5 is mixing at 15-25°C.

[0041] Preferably, the spray drying conditions in S5 are: inlet air temperature 120-200° C., outlet air temperature 60-100° C., and feed speed 4.5-36 g / min.

[0042] In the above-mentioned flavor-retaining flavor oil microcapsule powder, the solid fat and the wall material not only synergistically improve the water solubility of the flavor oil, reduce the volatilization of the flavor oil, and improve the embedding rate, oxidative stability and fluidity of the flavor oil; more importantly, they show a significant synergistic effect in the retention and release of aroma components, achieving long-term retention of aroma components and their controllable release. When the above-mentioned flavor-retaining flavor oil microcapsule powder is used as a seasoning for processed foods, the taste and aroma of the processed foods can be guaranteed. Therefore, the application of the above-mentioned flavor-retaining flavor oil microcapsule powder in the preparation of processed foods should be within the protection scope of the present invention.

[0043] The present invention has the following beneficial effects:

[0044] 1. The present invention uses solid fat that is solid at room temperature to replace part of the seasoning oil in the core material, and after emulsification, it is combined with the wall material to form a microcapsule powder. Compared with microcapsules made of traditional nanoemulsions, the present invention has the following obvious advantages: 1) The addition of solid fat increases the steric hindrance between droplets, and the storage stability at room temperature is significantly improved, and it is not easy to have unstable phenomena such as phase stratification, droplet flocculation, polymerization, and Austenosis; 2) The solid fat and the wall material synergistically improve the water solubility of the seasoning oil, reduce the volatilization of the seasoning oil, reduce the surface oil content of the microcapsule, and improve the embedding rate, oxidative stability and fluidity of the seasoning oil; 3) The solid fat and the wall material show significant synergistic effects in the retention and release of aroma components, achieving long-term retention of aroma components and their controllable release.

[0045] 2. The particle size of the flavor-retaining flavor oil microcapsule powder of the present invention is uniform and stable, and the microcapsule powder can be quickly formed during the spray drying process, with little loss of active ingredients, and the flavor oil can be effectively isolated from light, heat and oxygen, thereby greatly improving the stability of the flavor oil.

[0046] 3. The preparation process of the flavor-retaining flavoring oil microcapsule powder of the present invention is simple and suitable for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1The hydrogen peroxide values ​​of the products obtained in Examples 1 to 2 and Comparative Examples 1 to 6 are shown in FIG.

[0048] Figure 2 a is the aroma retention and release of the product obtained in Example 1 after being exposed for 0, 4, and 10 days, Figure 2 b is the aroma retention and release of the product obtained in Example 2 after being exposed for 0, 4, and 10 days. Figure 2 c is the aroma retention and release of the product obtained in comparative example 1 after being left open for 0, 4, and 10 days, Figure 2 d is the aroma retention and release of the product obtained in Comparative Example 2 after being left open for 0, 4, and 10 days. Figure 2 e is the aroma retention and release of the product obtained in comparative example 3 after being left open for 0, 4, and 10 days. Figure 2 f is the aroma retention and release of the product obtained in Comparative Example 4 after being left open for 0, 4, and 10 days, Figure 2 g is the aroma retention and release of the product obtained in comparative example 5 after being exposed for 0, 4, and 10 days, Figure 2 h is the aroma retention and release of the product obtained in Comparative Example 6 after being left open for 0, 4, and 10 days.

[0049] Figure 3 a is the aroma retention and release of the product obtained in Example 1 after 6 hours of heat preservation, Figure 3 b is the aroma retention and release of the product obtained in Example 2 after 6 hours of heat preservation, Figure 3 c is the aroma retention and release of the product obtained in Example 3 after being kept warm for 6 hours. DETAILED DESCRIPTION

[0050] The present invention is further described below in conjunction with the accompanying drawings and specific examples, but the examples do not limit the present invention in any form. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.

[0051] Unless otherwise specified, the reagents and materials used in the following examples are commercially available.

[0052] Example 1 Preparation of flavor-retaining flavor oil microcapsule powder

[0053] S1. 15 g of cocoa butter was heated at 45 ° C until completely melted, and then mixed with 15 g of mustard oil to obtain a core material;

[0054] S2. Add 3 g of Tween 80 to 116 mL of deionized water and stir at 45 °C for 10 min until dissolved to obtain an aqueous phase;

[0055] S3. Hydrate gum arabic and β-cyclodextrin in a mass ratio of 1:1 until they are completely dissolved to obtain a wall material solution;

[0056] S4. The core material and the aqueous phase with a mass ratio of 1:4 were stirred at a constant temperature of 45°C for 10 minutes, and then high-speed shear mixing was performed at 45°C and 10,000 rpm for 3 minutes, and homogenization was circulated for 6 times at 45°C and 500 bar, and then ice-water bathed at 4°C for 30 minutes to obtain an NLC emulsion;

[0057] S5. The wall material solution and the NLC emulsion are mixed at 15°C (the mass ratio of the wall material to the core material is controlled to be 3:1), and then spray-dried to obtain the flavor-retaining flavor oil microcapsule powder;

[0058] The spray drying conditions in S5 are as follows: an inlet air temperature of 130°C, an outlet air temperature of 60°C, and a feed speed of 20 g / min.

[0059] Example 2 Preparation of flavor-retaining flavor oil microcapsule powder

[0060] S1. 30 g of beeswax was heated at 75 ° C until completely melted, and then mixed with 15 g of pepper oil to obtain a core material;

[0061] S2. Add 6 g of soybean lecithin to 600 mL of deionized water and stir at 75 ° C for 10 min until dissolved to obtain an aqueous phase;

[0062] S3. Hydrate the modified starch until it is completely dissolved to obtain a wall material solution;

[0063] S4. The core material and the aqueous phase in a mass ratio of 1:9 were stirred at a constant temperature of 75°C for 10 min, and then high-speed shear mixed at 75°C and 8000 rpm for 10 min, ultrasonically crushed at 75°C and 500 W for 4 min, and cooled at 25°C for 20 min to obtain an NLC emulsion;

[0064] S5. The wall material solution and the NLC emulsion are mixed at 25°C (the mass ratio of the wall material to the core material is controlled to be 1:1), and then spray-dried to obtain the flavor-retaining flavoring oil microcapsule powder;

[0065] The spray drying conditions in S5 are as follows: an inlet air temperature of 120°C, an outlet air temperature of 60°C, and a feed speed of 4.5 g / min.

[0066] Example 3 Preparation of flavor-retaining flavor oil microcapsule powder

[0067] S1. 18 g of stearic acid was heated at 78 ° C until completely melted, and then mixed with 12 g of pepper oil to obtain a core material;

[0068] S2. Add 3 g of Tween 20 to 75 mL of deionized water and stir at 78 °C for 10 min until dissolved to obtain an aqueous phase;

[0069] S3. hydrating maltodextrin and gum arabic in a mass ratio of 1:2 until completely dissolved to obtain a wall material solution;

[0070] S4. The core material and the aqueous phase with a mass ratio of 3:7 were stirred at a constant temperature at 78°C for 10 minutes, and then high-speed shear mixing was performed at 78°C and 15000 rpm for 2 minutes, and homogenization was circulated for 3 times at 78°C and 1000 bar, and a water bath was performed at 20°C for 40 minutes to obtain an NLC emulsion;

[0071] S5. The wall material solution and the NLC emulsion are mixed at 15°C (the mass ratio of the wall material to the core material is controlled to be 6:1), and then spray-dried to obtain the flavor-retaining flavor oil microcapsule powder;

[0072] The spray drying conditions in S5 are as follows: an inlet air temperature of 200°C, an outlet air temperature of 100°C, and a feed speed of 36 g / min.

[0073] Comparative Example 1

[0074] Same as Example 1, except that cocoa butter is replaced by soybean oil.

[0075] Comparative Example 2

[0076] Same as Example 2, except that beeswax is replaced by soybean oil.

[0077] Comparative Example 3

[0078] Same as Example 1, except that only S1, S2 and S4 are performed, that is, the product is an NLC emulsion.

[0079] Comparative Example 4

[0080] Same as Example 1, except that cocoa butter is replaced by soybean oil; and only S1, S2 and S4 are performed, that is, the product is a nanoemulsion (that is, cocoa butter is replaced by soybean oil in the preparation process of the aforementioned NLC emulsion).

[0081] Comparative Example 5

[0082] Same as Example 2, except that only S1, S2 and S4 are performed, that is, the product is an NLC emulsion.

[0083] Comparative Example 6

[0084] Same as Example 2, except that beeswax is replaced by soybean oil; and only S1, S2 and S4 are performed, that is, the product is a nanoemulsion (that is, beeswax is replaced by soybean oil in the preparation process of the aforementioned NLC emulsion).

[0085] Comparative Example 7

[0086] The same as Example 1, except that in S4, the mass ratio of the core material to the aqueous phase is 2:3; and only S1, S2 and S4 are performed, that is, the product is an NLC emulsion.

[0087] In the preparation process of this comparative example, a stable NLC emulsion system cannot be formed, oil and water are separated, and a stable and uniform state cannot be maintained before spraying, so it is unnecessary to perform S3 and S5.

[0088] Comparative Example 8

[0089] The same as Example 1, except that in S5, the mass ratio of the wall material to the core material is 0.8:1.

[0090] The microcapsules prepared in this comparative example ruptured soon after the spraying was completed.

[0091] Comparative Example 9

[0092] Same as Example 1, except that, in S5, the mixing temperature is 5°C.

[0093] The microcapsules prepared in this comparative example ruptured soon after the spraying was completed.

[0094] Test Example 1

[0095] 1. Test Method

[0096] 1. Particle size and particle size distribution:

[0097] The particle size and particle size distribution of the products obtained in Examples 1 to 3, Comparative Examples 1 to 2 and Comparative Examples 8 to 9 were measured using a Mastersizer 3000 analyzer wet dispersion device. After adding the sample, the light shielding degree of the device was kept at 4% to 15%, and the volume weighted average diameter (D[4,3]) was measured. According to span = (d 90 -d 10 ) / d 50 (where d 90 d 50 and d 10 The particle size distribution span of the powder was calculated by using the volume diameters at 90%, 50% and 10% of the cumulative volume, respectively.

[0098] 2. Embedding rate:

[0099] Accurately weigh 1-2g (accurate to 0.001g, recorded as m0) of the products obtained in Examples 1-3, Comparative Examples 1-2 and Comparative Examples 8-9, respectively, and place them on folded filter paper, rinse the samples with 20mL of petroleum ether (boiling range 60-90°C) and filter, filter again after filtration, and repeat 3 times. Transfer the filtrate to a clean flask (m1), evaporate and recover the petroleum ether, and dry at 60°C to constant weight (m2). The total oil mass contained in 1g of product theoretically is recorded as m总 , then according to EE=[m0×m 总 -(m2-m1)] / (m0×m 总 )×100% to obtain the embedding efficiency EE.

[0100] 3. Moisture content:

[0101] First preheat the oven to 100±5℃, place a clean weighing bottle in the oven, and place the lid of the weighing bottle at an angle next to the weighing bottle. After turning on the oven and running for 2 hours, cover the weighing bottle, take it out and place it in a dryer, cool it to 25℃ and weigh it. Repeat the above steps until it is dried to a constant weight (i.e. the difference between the last two weights does not exceed 2 mg), and record the mass of the weighing bottle at this time as m0.

[0102] Accurately weigh 2 g (accurate to 0.001 g, recorded as m1) of the products obtained in Examples 1 to 3, Comparative Examples 1 to 2 and Comparative Examples 8 to 9, respectively, and place them in the aforementioned weighing bottles, and place the weighing bottles in an oven at 100±5°C, with the lids of the weighing bottles placed obliquely next to the weighing bottles. After turning on the oven and running for 2 hours, cover the weighing bottles, take them out and place them in a dryer, cool them to 25°C and weigh them, repeat the above steps until they are dried to constant weight (i.e., the difference between the last two weights does not exceed 2 mg), and record the total mass of the weighing bottle and the product as m2.

[0103] Finally, the moisture content is calculated according to moisture content = (m0 + m1 - m2) / m1 × 100%.

[0104] 4. Liquidity:

[0105] Weigh 10 g of the products obtained in Examples 1 to 3, Comparative Examples 1 to 2 and Comparative Examples 8 to 9, and allow the products to fall freely on a horizontal plate through a funnel to accumulate. The height H and the accumulation diameter D of the product accumulation were measured, and the angle of repose θ was calculated according to θ=arctan(2H / D) to evaluate the fluidity of the product.

[0106] 5. Oxidative stability:

[0107] The products obtained in Examples 1 to 2 and Comparative Examples 1 to 6 were first placed in an oven at 60° C. for accelerated oxidation for 10 days, and the oxidative stability was evaluated by measuring the hydrogen peroxide value of the products on days 0, 1, 2, 4, 6, 8, and 10. The specific method was as follows: 0.100 g of the products obtained in Examples 1 to 2 and Comparative Examples 1 to 2, and 0.3 mL of the products obtained in Comparative Examples 3 to 6 were respectively weighed in centrifuge tubes, 1.5 mL of isooctane / isopropanol mixed solution (3:1, v / v) was added to each tube, vortexed 3 times (each time for 10 s), and then centrifuged at 10000 r / min for 5 min, 200 μL of the supernatant was taken, and 2.8 mL of methanol / n-butanol mixed solution (2:1, v / v) was added to the supernatant. To form color, add 50 μL of ammonium thiocyanate and 50 μL of ferrous solution (mix 0.132 mol / L BaCl2 and 0.144 mol / L FeSO4, centrifuge at 10000 r / min for 5 min, and take the supernatant to obtain the ferrous solution) to the system, vortex the sample briefly for 4 seconds, equilibrate in the dark for 20 minutes, and finally measure the absorbance at 510 nm using an ultraviolet spectrophotometer. The amount of hydrogen peroxide produced by oil oxidation is calculated using the standard curve of cumene hydroperoxide.

[0108] 6. Aroma retention and release effect:

[0109] (1) Weigh 0.8 g (accurate to 0.01 g) of the products obtained in Examples 1 to 2 and Comparative Examples 1 to 2, and 2.4 mL (accurate to 0.01 mL) of the products obtained in Comparative Examples 3 to 6, respectively, and place them in an open headspace bottle for 0, 4, and 10 days. Then seal them with paraffin film and equilibrate for 6 hours. Then, an electronic nose is used to measure the flavor substances of the products and determine the flavor release, so as to evaluate the aroma retention and release effects of the products.

[0110] (2) Weigh 0.8 g (accurate to 0.01 g) of the products obtained in Examples 1 to 3, seal them with paraffin film, and keep them warm for 6 h in a temperature environment near the melting point of the solid fat used in the products (±7° C.) (to ensure that the volatile substances reach equilibrium in the air). The result of keeping them warm for 6 h at room temperature (25° C.) is used as a control. The flavor substances of the products are measured with an electronic nose to determine the release of the flavor, so as to evaluate the aroma retention and release effect of the products.

[0111] The parameters of the electronic nose were set as follows: gas flow rate 300 mL / min, data acquisition time 180 s, data acquisition delay time 100 s, manual headspace injection. Each sample was run in parallel 3 times. The names of the sensors in the electronic nose are shown in Table 1.

[0112] Table 1 Names of the sensors in the electronic nose

[0113] Array number Sensor Name Performance Description 1 W1C Aromatic ingredients, benzene 2 W5S High sensitivity, very sensitive to nitrogen oxides 3 W3C Sensitive aromatic ingredients, ammonia 4 W6S Mainly selective for hydrides 5 W5C Short chain alkane aromatic components 6 W1S Sensitive to methyl 7 W1W Sensitive to sulfide 8 W2S Sensitive to alcohols, aldehydes and ketones 9 W2W Aromatic ingredients, sensitive to organic sulfides 10 W3S Sensitive to long chain alkanes

[0114] 2. Test Results

[0115] 1. Physical properties measurement results

[0116] The embedding rate is an important indicator for evaluating the quality of microcapsule products. A high embedding rate means less core material exposed on the surface of the microcapsule, and less loss of effective ingredients. The smaller the angle of repose, the better the fluidity of the microcapsule, which is more conducive to storage and transportation. The results of the physical properties such as particle size, particle size distribution, embedding rate, moisture content, and repose angle of the products obtained from Examples 1 to 3, Comparative Examples 1 to 2, and Comparative Examples 8 to 9 are shown in Table 2.

[0117] Table 2 Physical properties test results

[0118] Group Particle size (μm) span Embedding rate (%) Moisture content (%) Angle of repose(°) Example 1 1.92±0.17 2.20±0.14 77.51±2.23 3.58±0.10 40.20±1.16 Example 2 2.65±0.00 2.01±0.03 79.79±1.31 3.01±0.12 38.40±0.06 Example 3 1.58±0.02 2.38±0.00 89.63±1.29 1.46±0.06 34.18±0.21 Comparative Example 1 4.53±1.74 4.99±0.48 71.75±1.82 3.88±0.07 41.26±1.01 Comparative Example 2 5.03±1.24 3.54±0.23 74.26±1.28 3.96±0.09 40.82±0.27 Comparative Example 8 14.25±1.13 32.81±6.30 20.89±0.21 4.08±0.11 43.77±0.28 Comparative Example 9 12.54±2.47 22.32±4.87 23.04±1.59 6.07±0.22 44.33±0.39

[0119] As can be seen from Table 2, the particle size, particle size distribution, moisture content and repose angle of the products obtained in Examples 1 to 3 are significantly lower than those in Comparative Examples 1 to 2 and Comparative Examples 8 to 9, and the embedding rate of the products obtained in Examples 1 to 3 is significantly higher than that in Comparative Examples 1 to 2 and Comparative Examples 8 to 9, indicating that it is the use of solid fat to replace part of the flavoring oil in the flavor-retaining flavoring oil microcapsule powder of the present invention, and the specific control of the amount of each raw material and the preparation process, that enables the flavor-retaining flavoring oil microcapsule powder to have a uniform particle size, better fluidity, lower moisture content and higher embedding rate.

[0120] 2. Oxidation stability test results

[0121] The hydrogen peroxide values ​​of the products obtained in Examples 1 to 2 and Comparative Examples 1 to 6 are as follows: Figure 1 shown.

[0122] Depend on Figure 1 It can be seen that:

[0123] (1) Compared with Comparative Examples 1 to 6, the hydrogen peroxide values ​​of Examples 1 to 2 are significantly reduced, and there is a significant difference, indicating that the aroma-retaining flavoring oil microcapsule powder of the present invention has excellent oxidative stability and can significantly extend the shelf life of the flavoring oil.

[0124] (2) The hydrogen peroxide value of the product obtained in Example 1 on the 10th day was only 2.21±0.10mmol / kg, while the hydrogen peroxide value of the comparative example 1 without adding solid fat on the 10th day reached 21.14±0.12mmol / kg, and even the hydrogen peroxide value on the 6th day was as high as 27.82±0.62mmol / kg, indicating that it is the use of solid fat in the present invention to replace part of the flavoring oil in the flavoring oil microcapsule powder that significantly improves the oxidative stability of the flavoring oil microcapsule powder.

[0125] (3) The hydrogen peroxide value of the product obtained in Example 2 on the 10th day was only 6.34±0.33mmol / kg, while the hydrogen peroxide value of the comparative example 2 without adding solid fat on the 10th day reached 26.43±0.59mmol / kg, indicating that it is the use of solid fat in the present invention to replace part of the flavoring oil in the flavor-retaining flavoring oil microcapsule powder that significantly improves the oxidative stability of the flavor-retaining flavoring oil microcapsule powder.

[0126] (4) In the first 4 days of accelerated oxidation, the oxidative stability of Comparative Example 3 was significantly better than that of Comparative Example 4. Then, the hydrogen peroxide value of Comparative Example 3 increased sharply and was basically the same as that of Comparative Example 4 on the 6th day, indicating that the addition of solid fat can only provide protection for the oil in the early stage of oxidation, that is, the long-term oxidative stability of the flavor-retaining flavor oil microcapsule powder of the present invention is the result of the synergistic effect of the wall material and the solid fat, rather than the effect of a single component.

[0127] (5) The hydrogen peroxide value of the product obtained in Example 2 on the 10th day was only 6.34±0.33 mmol / kg, while the hydrogen peroxide value of the comparative example 5 without using the wall material on the 10th day reached 36.24±1.69 mmol / kg, indicating that the wall material is crucial to the oxidative stability of the flavor-retaining flavoring oil microcapsule powder of the present invention.

[0128] (6) There is no significant difference in hydrogen peroxide value between Comparative Example 5 and Comparative Example 6, indicating that the long-term oxidative stability of the aroma-retaining flavoring oil microcapsule powder of the present invention is the result of the synergistic effect of the wall material and the solid fat, rather than the effect of a single component.

[0129] 3. Aroma retention and release effect test results

[0130] Since the fragrance-retaining ingredients are easily lost during processing or storage, the fragrance-retaining effect is also a key indicator for evaluating the quality of microcapsule products. As time goes by, the ideal fragrance-retaining microcapsules should show the effect of slowly releasing fragrance during storage.

[0131] (1) The aroma retention and release of the products obtained in Examples 1 to 2 and Comparative Examples 1 to 6 after being left open for 0, 4, and 10 days are shown in the following table. Figure 2 As shown, Figure 2 a is the aroma retention and release of the product obtained in Example 1 after being exposed for 0, 4, and 10 days, Figure 2 b is the aroma retention and release of the product obtained in Example 2 after being exposed for 0, 4, and 10 days. Figure 2 c is the aroma retention and release of the product obtained in comparative example 1 after being left open for 0, 4, and 10 days, Figure 2 d is the aroma retention and release of the product obtained in Comparative Example 2 after being left open for 0, 4, and 10 days. Figure 2 e is the aroma retention and release of the product obtained in comparative example 3 after being left open for 0, 4, and 10 days. Figure 2 f is the aroma retention and release of the product obtained in Comparative Example 4 after being left open for 0, 4, and 10 days, Figure 2 g is the aroma retention and release of the product obtained in comparative example 5 after being exposed for 0, 4, and 10 days, Figure 2 h is the aroma retention and release of the product obtained in Comparative Example 6 after being left open for 0, 4, and 10 days.

[0132] Depend on Figure 2 It can be seen that the aroma retention and release effects of the products obtained in Examples 1 to 2 are good. As the storage time increases, the radar graph profiles are basically consistent, the response values ​​of each sensor do not change significantly, and a distinct characteristic aroma can be smelled. However, the aroma of the products obtained in Comparative Examples 1 to 6 weakens as the storage time increases, and the radar graph profiles show obvious differences, that is, there is a serious aroma loss phenomenon during the storage period, and the characteristic aroma can hardly be smelled in the later period.

[0133] This indicates that the aroma-retaining flavor oil microcapsule powder of the present invention achieves long-term retention of aroma components, while the flavor oil of the product obtained in the comparative example has a sudden release of aroma and is not well protected.

[0134] (2) The aroma retention and release of the products obtained in Examples 1 to 3 after 6 hours of heat preservation are as follows Figure 3 As shown, Figure 3 a is the aroma retention and release of the product obtained in Example 1 after 6 hours of heat preservation, Figure 3 b is the aroma retention and release of the product obtained in Example 2 after 6 hours of heat preservation, Figure 3 c is the aroma retention and release of the product obtained in Example 3 after being kept warm for 6 hours.

[0135] Depend on Figure 3 It can be seen that when the products obtained in Examples 1 to 3 are placed in an environment near the melting point of solid fat (±7°C), the aroma release intensity of the products is significantly enhanced, indicating that the aroma-retaining flavoring oil microcapsule powder of the present invention is temperature-sensitive and can achieve a burst release of aroma at a specific temperature, thereby achieving the effect of controlled release of aroma.

[0136] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A flavor-retaining flavoring oil microcapsule powder, characterized in that: It is made of NLC emulsion and wall material, wherein the NLC emulsion comprises a core material and an aqueous phase in a mass ratio of 1 to 3:7 to 9; the aqueous phase comprises an emulsifier and water, and the mass concentration of the emulsifier in the aqueous phase is 1 to 4%; the mass ratio of the core material to the wall material is 1:1 to 6; the core material comprises a solid fat and a seasoning oil in a mass ratio of 1 to 36:4, and the solid fat is a solid fat with a melting point above 35°C; the solid fat comprises one or more of cocoa butter, beeswax, and stearic acid, and the seasoning oil comprises one or more of mustard oil, vine pepper oil, and prickly ash oil; the wall material is one or more of maltodextrin, modified starch, gum arabic, and β-cyclodextrin; the emulsifier is one or more of Tween 20, Tween 80, and soybean lecithin; The preparation method of the fragrance-retaining flavoring oil microcapsule powder comprises the following steps: S1. After the solid fat is heated until completely melted, it is mixed with the seasoning oil to obtain a core material; S2. dissolving the emulsifier in water to obtain an aqueous phase; S3. Hydrate the wall material until it is completely dissolved to obtain a wall material solution; S4. The core material obtained in S1 and the aqueous phase obtained in S2 are mixed and sheared, homogenized or ultrasonicated, and then cooled to obtain an NLC emulsion; S5. After mixing the wall material solution obtained from S3 and the NLC emulsion obtained from S4, spray drying was performed to obtain the flavor-type seasoning oil microcapsule powder; Among them, the shearing described in S4 is shearing at 8000-15000rpm for 2-10min; the homogenization described in S4 is homogenization at 500-1000bar for 3-7 times; the mixing temperature described in S4 is more than 5°C higher than the melting point of the solid fat; the mixing described in S5 is mixing at 15-25°C; the spray drying conditions described in S5 are: inlet air temperature 120-200°C, outlet air temperature 60-100°C, feed rate 4.5-36g / min; and the execution order of S1, S2, and S3 is not limited.

2. Use of the aroma-retaining flavoring oil microcapsule powder according to claim 1 in the preparation of processed foods.

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