A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages

Abstract

This invention relates to the field of beverage stability assessment technology. To address the problems of existing methods for evaluating the suspension performance and processing tolerance of colloidal microcrystalline cellulose in neutral milk beverages, which involve large workloads, high raw material requirements, high-level equipment, and long evaluation cycles, easily leading to a loss of product competitiveness, this invention discloses a rapid method for evaluating the application performance of colloidal microcrystalline cellulose in neutral milk beverages. The method evaluates the colloidal microcrystalline cellulose by detecting the dry powder particle size d(0.9) and D[4,3] of the tested colloidal microcrystalline cellulose, and by detecting the centrifugation sedimentation rate, oil bath tolerance time, and pouring score after oil bath in the mixture containing the tested colloidal microcrystalline cellulose. This method can quickly determine the processing suitability of microcrystalline cellulose in neutral milk beverages, providing theoretical guidance and basis for production applications. The short evaluation time can effectively shorten the product development cycle, and the method has low equipment requirements and is easy to operate.

Description

Technical Field

[0001] This invention relates to the field of beverage stability assessment technology, and in particular to a method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral milk beverages. Background Technology

[0002] Milk is widely recognized as a healthy and high-quality food due to its rich protein content and easily digestible calcium caseinate and calcium phosphate. Neutral milk beverages are liquid dairy products made primarily from fresh or reconstituted milk, with the addition of water, sugar, and other ingredients, processed through pasteurization or ultra-high temperature (UHT) sterilization. Neutral milk beverages hold a significant position in the beverage market and their market size is increasing year by year. Among them, UHT-sterilized PET bottle-packaged neutral milk beverages are a key product category for many dairy and beverage companies due to their lack of susceptibility to temperature and refrigeration requirements and their extended sales radius and cycle. However, neutral milk beverages typically contain some insoluble or oil-soluble components that exist in a dispersed state within the system, providing corresponding taste, nutrition, or function, such as cocoa powder, matcha, plant fiber, and fat. However, because the density of the aforementioned components differs from that of the dispersion medium in the system, or because these components are difficult to disperse uniformly in the system, neutral milk beverages often experience fat floating, stratification, flocculation, or sedimentation during processing or shelf life under the influence of gravity or mechanical forces. To address these issues, constructing a suitable suspension system for neutral milk beverages has become a key research focus for beverage developers. In neutral milk beverages, stabilizers such as microcrystalline cellulose, gellan gum, and agar are commonly used to provide suspension properties and construct a stable system. Among these, microcrystalline cellulose is widely used due to its strong processing tolerance, good suspension properties, ease of availability, and low cost.

[0003] Microcrystalline cellulose is a linear polysaccharide linked by β-1,4-glucosidic bonds. It is a white, odorless, and tasteless crystalline powder composed of extremely fine, free-flowing, rod-shaped or powdery porous particles obtained by hydrolyzing natural cellulose with dilute acid to its limiting degree of polymerization. The degree of polymerization of microcrystalline cellulose is typically much greater than 1000, and it is not digested or absorbed by the human body. The colloidal grade of microcrystalline cellulose used as a stabilizer is 0.1-2 μm. However, the performance of colloidal microcrystalline cellulose stabilizers from different manufacturers and of different models varies due to differences in raw material sources, production processes, and the type, molecular weight, and degree of substitution of dispersants. Furthermore, the wide range of solution particle sizes (0.1-2 μm) leads to significant differences in suspension properties, weak gelation degree, and processing tolerance during application, thus affecting the final state and quality of the product.

[0004] To evaluate whether a particular type of colloidal microcrystalline cellulose meets the requirements for processing tolerance, suspension capacity, and absence of significant weak gelation during shelf life in neutral dairy beverages, the current approach typically involves applying it to a specific product using appropriate dosage and processing methods. This is followed by extensive shelf-life monitoring or the use of various instruments for testing. For example, Zeng Wenbing et al. evaluated the effect of microcrystalline cellulose-containing stabilizers on the stability of high-calcium cocoa milk in their study, "Study on the effect of compound emulsifying stabilizers containing colloidal microcrystalline cellulose on the stability of high-calcium cocoa milk." This method requires testing a series of indicators, including the rheological properties of the finished product, Lumisizer stability, Turbiscan scanning, and changes in weak gelation during shelf life. It involves a huge workload, demands sophisticated equipment, and leads to significant waste of food raw materials due to continuous experimentation. Most importantly, the long shelf-life monitoring period significantly extends the beverage development cycle. Since beverages are fast-moving consumer goods, rapid product updates and replacements mean that a prolonged R&D cycle can directly lead to a product losing competitiveness or even failing to survive in the market. In order to reduce waste, overcome instrument limitations, shorten the R&D cycle, improve R&D efficiency, seize market opportunities, and enhance product competitiveness, it is necessary to establish a method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages. Summary of the Invention

[0005] To overcome the problems of existing methods for evaluating the suspension properties and processing tolerance of colloidal microcrystalline cellulose in neutral milk beverages, such as large workload, high demand for raw materials and auxiliary materials, high-level equipment, and long evaluation cycles, which can easily lead to loss of product competitiveness, this invention provides a method for rapidly evaluating the application performance of colloidal microcrystalline cellulose in neutral milk beverages. This method can quickly determine the processing suitability of microcrystalline cellulose in neutral milk beverages, providing theoretical guidance and basis for production applications. The short evaluation time can effectively shorten the product development cycle and enhance product competitiveness. Furthermore, this method has low equipment requirements and is easy to operate.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages includes the following steps:

[0008] (1) The dry powder particle size d (0.9) and D [4,3] of the colloidal microcrystalline cellulose to be tested were detected;

[0009] (2) Add the colloidal microcrystalline cellulose powder to be tested to water, shear and homogenize to obtain a mixture;

[0010] (3) Centrifuge the mixture obtained in step (2), dry the precipitate obtained by centrifugation, weigh it, and calculate the centrifugation precipitation rate;

[0011] (4) Add the mixture obtained in step (2) to a sealed container and then treat it with an oil bath. Stop the oil bath when one or more non-uniform states such as stratification, water separation, agglomeration, flocculation, and particle adhesion appear. Record the oil bath time as the oil bath tolerance time.

[0012] (5) After the oil bath treatment, the mixture is naturally cooled and then poured out. Its smoothness is scored to obtain a pouring score.

[0013] (6) Evaluation was conducted by dry powder particle size, centrifugal sedimentation rate, oil bath tolerance time, and pouring score.

[0014] This invention utilizes multiple indicators, including dry powder particle size, centrifugal sedimentation rate of a 1% microcrystalline cellulose solution, oil bath tolerance time, and pouring score after an oil bath, to comprehensively assess the suspension, processing tolerance, and weak gelation degree of colloidal microcrystalline cellulose in neutral milk beverages. This allows for a more accurate evaluation of the application performance of colloidal microcrystalline cellulose in neutral milk beverages, enabling rapid screening of suitable colloidal microcrystalline cellulose for processing, suspension, and shelf-life storage in neutral milk beverages. This provides theoretical guidance and a basis for production applications, avoiding quality problems in neutral milk beverage products caused by stabilizers. This invention uses a small sample of colloidal microcrystalline cellulose, combined with indicators such as dry powder particle size, centrifugal sedimentation rate of a 1% microcrystalline cellulose solution, oil bath tolerance time, and pouring score after an oil bath, instead of directly adding colloidal microcrystalline cellulose to neutral milk beverages to produce a finished product. The application performance of colloidal microcrystalline cellulose in neutral milk beverages is evaluated by testing a series of indicators, including the rheological properties, Lumisizer stability, Turbiscan scan, and weak gelation changes during shelf life. The evaluation process requires only about 5g of colloidal microcrystalline cellulose, a small amount that is not limited by insufficient raw material availability. The entire evaluation process does not require the addition of other raw materials or auxiliary materials used in neutral dairy beverages, thus avoiding limitations caused by a lack of these materials. Furthermore, this invention replaces UHT sterilization equipment, expensive and scarce rheometers, Lumisizer stability analyzers, and Turbiscan stability scanners with conventional equipment such as centrifuges, particle size analyzers, and oil baths, significantly reducing the requirements for R&D equipment. Moreover, the indicators used in this invention are rapidly measured, greatly reducing the workload and time required for product preparation and stability evaluation verification. Finally, this invention comprehensively evaluates the application performance of colloidal microcrystalline cellulose in neutral dairy beverages through multiple indicators, including dry powder particle size, centrifugation sedimentation rate of a 1% microcrystalline cellulose solution, oil bath tolerance time, and post-oil bath pouring score, enabling rapid screening of colloidal microcrystalline cellulose suitable for neutral dairy beverage processing.

[0015] Preferably, the water temperature in step (2) is room temperature, and the mass concentration of the colloidal microcrystalline cellulose to be tested in the mixture is 1%.

[0016] The particle size of colloidal microcrystalline cellulose and the proportion of non-colloidal microcrystalline cellulose precipitated by centrifugation directly affect the compactness and strength of the three-dimensional network structure formed after dispersion in the continuous phase. This directly reflects the suspending capacity that microcrystalline cellulose can provide to the system. The magnitude of the suspending capacity determines whether the particles in the neutral dairy beverage system can be uniformly dispersed, directly affecting the appearance quality of the product. This invention uses the centrifugation sedimentation rate of a 1% microcrystalline cellulose solution as an indicator. The 1% mass concentration is much higher than the amount of microcrystalline cellulose added in the neutral dairy beverage formulation. Scale-up the amount of microcrystalline cellulose used can shorten the detection time and achieve rapid evaluation. Furthermore, the behavior of microcrystalline cellulose at the increased concentration is the same as that at low concentration under the detection conditions. Therefore, the evaluation results of the 1% microcrystalline cellulose solution can be used to evaluate microcrystalline cellulose in neutral dairy beverages.

[0017] Preferably, the shearing conditions in step (2) are 2500-3000 rpm, the shearing time is 20-30 min, the primary pressure of the homogenization is 200-300 bar, and the secondary pressure is 40-60 bar.

[0018] Preferably, the centrifugation conditions in step (3) are: 4000-5000 rpm, 20-30 min; and the drying conditions are: 40-60℃, 6-12 h.

[0019] Preferably, the centrifugal sedimentation rate (%) in step (3) is (m2-m1) / m×100, where m1 is the weight of the centrifuge tube, m is the mass of the mixture in the centrifuge tube, and m2 is the mass of the precipitate after drying.

[0020] The centrifugal sedimentation rate is the proportion of colloidal microcrystalline cellulose precipitated after centrifugation to all colloidal microcrystalline cellulose in the solution. Colloidal microcrystalline cellulose powder itself contains bound water. Therefore, when removing the water bound to the solution from the precipitate obtained by centrifugation, it is necessary to ensure that the dried microcrystalline cellulose is in the same state as the colloidal microcrystalline cellulose powder to be tested. Therefore, the drying temperature should not be too high to avoid removing the bound water in the colloidal microcrystalline cellulose, which would result in a lower centrifugal sedimentation rate than the actual value.

[0021] Preferably, the oil bath temperature in step (4) is 130°C.

[0022] The particle size of dry powder and the oil bath tolerance time can reflect the heat sterilization tolerance of colloidal microcrystalline cellulose during processing. Since most neutral dairy beverages are room-temperature, long-shelf-life drinks, and are rich in nutrients, they are highly susceptible to microbial growth during shelf life. To ensure product safety, ultra-high temperature sterilization is generally required. Ultra-high temperature sterilization affects all components of the product, especially colloidal microcrystalline cellulose, which plays a crucial role in stabilizing the product system. This invention, through extensive experiments, found that the particle size of colloidal microcrystalline cellulose dry powder and the oil bath tolerance time at 130℃ can directly reflect the heat tolerance of colloidal microcrystalline cellulose during production and processing. The particle size directly affects the heat-receiving area. When the particle size D[4,3] of colloidal microcrystalline cellulose dry powder is <55μm, the heat-receiving area is too large, making it unable to withstand heat sterilization during processing. The 130℃ oil bath test further simulates heat sterilization during production. Both conditions, when considered simultaneously, can accurately and quickly assess the heat tolerance of colloidal microcrystalline cellulose during the processing of neutral dairy beverages.

[0023] Preferably, step (4) involves taking 50-60g of the mixture obtained in step (2) and adding it to a 100mL pressure-resistant and heat-resistant bottle. After sealing the pressure-resistant and heat-resistant bottle, it is heated in an oil bath at 130°C. Once one or more non-uniform states such as stratification, water separation, agglomeration, flocculation, and particle adhesion to the wall appear, the oil bath is stopped, and the oil bath time is recorded as the oil bath tolerance time. The pressure-resistant and heat-resistant bottle has a tolerance pressure of 5-6 bar and a tolerance temperature of 140-180°C.

[0024] When testing the oil bath resistance of the mixture in a closed environment, adding 50-60g of the mixture to a 100mL pressure-resistant and heat-resistant bottle can ensure that the pressure in the pressure-resistant and heat-resistant bottle is below 5bar during the oil bath process, thereby avoiding the explosion of the pressure-resistant and heat-resistant bottle and ensuring test safety.

[0025] Preferably, the natural cooling in step (5) is air cooling under room temperature conditions while the object is in a static state; the pouring flow rate is 0.05 to 0.08 m / s.

[0026] Weak gels are very fragile and easily disappear after shaking, so they should be left to stand and shaken away before pouring and scoring.

[0027] As a preferred option, the pouring scoring criteria in step (5) are: Excellent - smooth pouring, with a uniform water flow diameter when pouring stably; Poor - uneven water flow diameter when pouring stably, with obvious weak gel formation.

[0028] Oil bath pour scoring serves as an alternative to assessing weak gelation during product shelf-life tracking. The presence of significant weak gelation not only affects the overall uniformity and stability of the product's contents on the shelf but also severely impacts its taste, making it a crucial indicator. The amount of weak gelation affects the fluidity of the solution; therefore, the degree of weak gelation in the mixture can be characterized by the smoothness of pouring at a constant pouring rate after an oil bath. Through shelf-life tracking of multiple neutral dairy beverages and evaluation using a combination of oil bath and traditional methods, it was found that pouring at a 130°C oil bath for at least 40 minutes provides a direct and rapid reflection of the degree of weak gelation over a 9-month shelf life. This method, by accelerating the chemical reaction through high temperature, significantly shortens the assessment cycle for weak gelation. Extensive experimental verification demonstrates the accuracy and reliability of this method, making it highly valuable for application.

[0029] As a preferred option, the evaluation criteria for step (6) are:

[0030] When the particle size of the dry colloidal microcrystalline cellulose powder to be tested is 55μm≤D[4,3]≤70μm and d(0.9)≤150μm, the centrifugal sedimentation rate is ≤10%, the oil bath tolerance time is ≥40min and the pouring score is excellent, the colloidal microcrystalline cellulose to be tested has good suspension performance and processing tolerance performance, and is not easy to self-aggregate to form a weak gel.

[0031] When the particle size D[4,3] of the dry colloidal microcrystalline cellulose powder to be tested is <55μm and the oil bath tolerance time is <40min, the processing tolerance of the colloidal microcrystalline cellulose to be tested is poor.

[0032] When the particle size D[4,3] of the dry colloidal microcrystalline cellulose powder to be tested is >70μm and the centrifugal sedimentation rate is >10%, the suspension performance of the colloidal microcrystalline cellulose is poor.

[0033] When the pouring score of the colloidal microcrystalline cellulose to be tested is poor, the colloidal microcrystalline cellulose to be tested is prone to self-aggregation and has strong weak gelation properties.

[0034] Only when the dry powder particle size, centrifugal sedimentation rate, oil bath tolerance time, and oil bath solution pouring score all meet the requirements can colloidal microcrystalline cellulose ensure that it meets the needs of the production, processing, and storage of neutral dairy beverages in PET packaging. Colloidal microcrystalline cellulose dry powder with a particle size of 55μm≤D[4,3]≤70μm and d(0.9)≤150μm, a centrifugal sedimentation rate≤10%, an oil bath tolerance time≥40min, and an excellent pouring score indicates that the colloidal microcrystalline cellulose has good suspension capacity, can withstand the sterilization process of neutral dairy beverages in PET packaging, and will not exhibit significant weak gelation during shelf life, resulting in good sensory quality. When the colloidal microcrystalline cellulose dry powder particle size D[4,3]<55μm and the oil bath tolerance time<40min, due to the smaller particle size and increased surface area for the same mass, it is subjected to more heat during production and processing, leading to poorer processing tolerance and making it difficult to pass the sterilization process of neutral dairy beverages in PET packaging. Production and processing of neutral milk beverages; When the particle size D[4,3] of colloidal microcrystalline cellulose dry powder is greater than 70 μm and the centrifugal sedimentation rate is greater than 10%, due to the large particle size of colloidal microcrystalline cellulose, even after homogenization, some microcrystalline cellulose particles are still larger than 0.1 μm after forming a solution, which leads to a significant decrease in the elastic modulus that microcrystalline cellulose can provide. When applied, the suspending force is weak and it cannot properly suspend some particles in neutral milk beverages. Therefore, it is difficult to ensure that the neutral milk beverage maintains a uniform and stable overall state during the shelf life; A pouring score of poor indicates that the microcrystalline cellulose is very likely to further aggregate with fiber, protein and other components in the neutral milk beverage system during the shelf life, forming a weak gel. The weak gel seriously affects the taste and overall quality of the product.

[0035] Therefore, the present invention has the following beneficial effects:

[0036] (1) Only about 5g of colloidal microcrystalline cellulose raw material is needed to fully evaluate the application performance of the colloidal microcrystalline cellulose to be tested. The amount of raw material required is small and will not cause experimental limitations due to insufficient raw material.

[0037] (2) The entire evaluation process only requires colloidal microcrystalline cellulose as a raw material, without the need for other complex raw and auxiliary materials in the production and preparation of neutral milk beverages. It is not limited by the shortage of raw materials and the conclusions obtained from the evaluation are universally applicable to neutral milk beverages.

[0038] (3) Using the particle size of microcrystalline cellulose, the centrifugation sedimentation rate of 1% microcrystalline cellulose solution, the oil bath tolerance time, and the pouring score after the oil bath as indicators, the suspension ability, processing tolerance and weak gelation degree of the microcrystalline cellulose to be tested can be quickly and comprehensively evaluated without the need to prepare it into a neutral milk beverage product, saving a lot of time and manpower and greatly reducing the workload.

[0039] (4) The equipment used for testing indicators is common and readily available, simple to operate and has low environmental requirements, eliminating the food processing site and equipment restrictions required for the preparation of neutral milk beverage products, and also eliminating the restrictions of expensive and uncommon instruments and professional operators required for the testing of stability indicators of beverage products.

[0040] (5) Rapid and efficient screening of colloidal microcrystalline cellulose raw materials provides guidance for product development, greatly shortens the product development cycle, and enhances the product's market competitiveness. Detailed Implementation

[0041] The present invention will be further described below with reference to specific implementation methods.

[0042] In the following specific implementation method, the particle size analyzer used for measuring particle size was purchased from Malvern Ltd., UK, model Mastersizer3000. The particle size detection conditions were: air, pressure 2.5 bar, vibration rate 75%. The shearing equipment was a high-speed shearing machine purchased from Silverson Ltd., UK, model L5M.

[0043] The scoring criteria for pouring are shown in the table below. The lower the score, the stronger the suspension ability and stability of the tested microcrystalline cellulose. A score of 0-4 indicates an excellent pouring score, meaning smooth pouring. When the pouring angle is fixed and the pouring flow rate is stable, the diameter of the water flow after stable pouring is uniform. This indicates that the mixture after oil bath treatment has not formed a weak gel or has formed a small amount of weak gel that does not affect the flow of the mixture. However, when the pouring score is ≥5, the diameter of the water flow is not uniform during stable pouring, resulting in an inferior pouring score. Furthermore, as the score increases, the weak gel gradually strengthens, leading to a decrease in the smoothness of pouring or even the inability to pour.

[0044]

[0045] Example 1

[0046] A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages includes the following steps:

[0047] (1) Weigh 2g of colloidal microcrystalline cellulose powder sample 1#, and use Malvern Mastersizer 3000 laser particle size analyzer to detect the particle size distribution of the dry powder. Record the particle size detection values ​​d(0.9)=127.26μm and D[4,3]=62.94μm;

[0048] (2) Add 1g of colloidal microcrystalline cellulose to 100g of room temperature water, shear at 2500rpm for 20min to disperse it evenly, and after stopping the shearing, homogenize it under the conditions of first-stage pressure of 200bar and second-stage pressure of 40bar to obtain mixture A;

[0049] (3) Centrifuge 50g of mixture A at 4000rpm for 20min, discard the supernatant, dry the precipitate at 60℃ for 6h and weigh it. The centrifugation precipitation rate of mixture A is calculated to be 5%.

[0050] (4) Place 50g of mixture A into a 100mL pressure-resistant and heat-resistant bottle and treat it in an oil bath at 130℃ to obtain B. The time required for slight water separation on the surface of B is 60min.

[0051] (5) Take out B while keeping it stable. After it cools down naturally, pour it out and score its smoothness. A score of 3 points is considered excellent.

[0052] (6) Evaluation of sample #1: The dry powder particle size is 55μm≤D[4,3]=62.94μm≤70μm and d(0.9)=127.26μm≤150μm, the centrifugal sedimentation rate is 5%≤10%, the oil bath tolerance time is 60min≥40min and the pouring score is excellent. This indicates that the colloidal microcrystalline cellulose has good suspension ability and can withstand the sterilization process of neutral milk beverages in PET packaging. Furthermore, there will be no obvious weak gelation during the shelf life, and the product has good sensory quality.

[0053] The colloidal microcrystalline cellulose 1# evaluated in Example 1 was used in the actual production of cocoa-flavored milk beverage. The resulting cocoa-flavored milk beverage was in good condition and remained uniform and stable throughout the entire shelf life without any obvious weak gelation.

[0054] Example 2

[0055] A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages includes the following steps:

[0056] (1) Weigh 2g of colloidal microcrystalline cellulose powder sample 2#, and use Malvern Mastersizer 3000 laser particle size analyzer to detect the particle size distribution of the dry powder. Record the particle size detection values ​​d(0.9)=147.31μm and D[4,3]=57.84μm;

[0057] (2) Add 3g of 2# colloidal microcrystalline cellulose to 300g of room temperature water, shear at 3000rpm for 30min to disperse it evenly, and after stopping the shearing, homogenize it under the conditions of first-stage pressure of 250bar and second-stage pressure of 50bar to obtain mixture A;

[0058] (3) Centrifuge 50g of mixture A at 5000rpm for 30min, discard the supernatant, dry the precipitate at 50℃ for 8h and weigh it. The centrifugation precipitation rate of mixture A is calculated to be 7%.

[0059] (4) Place 50g of mixture A into a 100mL pressure-resistant and heat-resistant bottle and treat it in an oil bath at 130℃ to obtain B. The time required for slight aggregation in the middle of B is 52min.

[0060] (5) Take out B while keeping it stable. After it cools down naturally, pour it out and score its smoothness. A score of 2 points is considered excellent.

[0061] (6) Evaluation of sample #2: The dry powder particle size is 55μm≤D[4,3]=57.84μm≤70μm and d(0.9)=147.31μm≤150μm, the centrifugal sedimentation rate is 7%≤10%, the oil bath tolerance time is 52min≥40min and the pouring score is excellent. This indicates that the colloidal microcrystalline cellulose has good suspension ability and can withstand the sterilization process of neutral milk beverages in PET packaging. Furthermore, there will be no obvious weak gelation during the shelf life, and the product has good sensory quality.

[0062] The No. 2 colloidal microcrystalline cellulose evaluated in Example 2 was used in the actual production of high-calcium milk beverage. The resulting high-calcium milk beverage was in good condition and was uniformly stable throughout the shelf life without obvious weak gelation.

[0063] Example 3

[0064] A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages includes the following steps:

[0065] (1) Weigh 2g of colloidal microcrystalline cellulose powder sample 3#, and use Malvern Mastersizer 3000 laser particle size analyzer to detect the particle size distribution of the dry powder. Record the particle size detection values ​​d(0.9)=176.32μm and D[4,3]=69.33μm;

[0066] (2) Add 3g of 3# colloidal microcrystalline cellulose to 300g of room temperature water, shear at 3000rpm for 30min to disperse it evenly, and after stopping the shearing, homogenize it under the conditions of first-stage pressure of 250bar and second-stage pressure of 50bar to obtain mixture A;

[0067] (3) Centrifuge 50g of mixture A at 5000rpm for 30min, discard the supernatant, dry the precipitate at 60℃ for 6h and weigh it to obtain a centrifugation precipitate of 12% of mixture A.

[0068] (4) Put 50g of mixture A into a 100mL pressure-resistant and heat-resistant bottle and treat it in an oil bath at 130℃ to obtain B. The time required for a small amount of precipitate to appear at the bottom of B is 57min.

[0069] (5) Take out B while keeping it stable. After it cools down naturally, pour it out and score its smoothness. A score of 2 points is considered excellent.

[0070] (6) Evaluation of sample #3: Dry powder particle size 55μm≤D[4,3]=69.33μm≤70μm but d(0.9)=176.32μm>150μm, centrifugal sedimentation rate=12%>10%, oil bath tolerance time=57min≥40min and the pouring score is excellent. This indicates that the colloidal microcrystalline cellulose can withstand the sterilization process of neutral milk beverages in PET packaging and will not have obvious weak gelation during the shelf life. However, the suspension ability is poor and cannot guarantee the uniformity and stability of the neutral milk beverage particles.

[0071] When the colloidal microcrystalline cellulose evaluated in Example 3 was used in the actual production of oat-flavored milk beverage, the resulting oat-flavored milk beverage had a lot of sediment at the bottom, indicating that the colloidal microcrystalline cellulose could not meet the suspension requirements of oat-flavored milk beverage processing, and its use would seriously affect the sensory quality of neutral milk beverage.

[0072] Example 4

[0073] A method for rapidly evaluating the performance of colloidal microcrystalline cellulose in neutral dairy beverages includes the following steps:

[0074] (1) Weigh 2g of colloidal microcrystalline cellulose powder sample 4#, and use Malvern Mastersizer 3000 laser particle size analyzer to detect the particle size distribution of the dry powder. Record the particle size detection values ​​d(0.9)=100.13μm and D[4,3]=45.23μm;

[0075] (2) Add 3g of 4# colloidal microcrystalline cellulose to 300g of room temperature water, shear at 3000rpm for 30min to disperse it evenly, and after stopping the shearing, homogenize it under the conditions of first-stage pressure of 250bar and second-stage pressure of 50bar to obtain mixture A;

[0076] (3) Centrifuge 50g of mixture A at 5000rpm for 30min, discard the supernatant, dry the precipitate at 60℃ for 6h and weigh it to obtain 6% of the centrifuged precipitate of mixture A.

[0077] (4) Place 50g of mixture A into a 100mL pressure-resistant and heat-resistant bottle and treat it in an oil bath at 130℃ to obtain B. The time required for slight aggregation in the middle of B is 33min.

[0078] (5) Take out B while keeping it stable. After it cools down naturally, pour it out and score its smoothness. A score of 4 points is excellent.

[0079] (6) Evaluation of sample #4: Dry powder particle size d(0.9)=100.13μm≤150μm but D[4,3]=45.23μm<55μm, centrifugal sedimentation rate=6%≤10%, pouring score is excellent, but oil bath tolerance time=33min<40min, indicating that the colloidal microcrystalline cellulose has good suspension ability and no obvious weak gelation will appear during the shelf life, but it cannot tolerate the sterilization process of neutral milk beverages in PET packaging.

[0080] When the colloidal microcrystalline cellulose evaluated in Example 4 was used in the actual production of cocoa-flavored milk beverage, the resulting cocoa-flavored milk beverage directly flocculated and separated, indicating that the colloidal microcrystalline cellulose could not meet the normal processing requirements of cocoa-flavored milk beverage.

[0081] The evaluation results of colloidal microcrystalline cellulose in the above embodiments and the actual performance of colloidal microcrystalline cellulose in various types of neutral milk beverages show that the evaluation results obtained by the method of the present invention are consistent with the product suspension, processing tolerance and weak gelation results during actual production. This proves that the method of the present invention can effectively evaluate the application performance of colloidal microcrystalline cellulose in neutral milk beverages and can be used as a basis for screening colloidal microcrystalline cellulose with good performance in neutral milk beverages.

Claims

1. A method for rapidly evaluating the performance of colloidal grade microcrystalline cellulose in neutral milk beverages, characterized by, The method comprises the following steps: (1) detecting the dry powder particle size d(0.9) and D[4,3] of the colloidal microcrystalline cellulose to be tested; (2) adding the colloidal microcrystalline cellulose dry powder to be tested into water, shearing and homogenizing to obtain a mixed solution, and the mass concentration of the colloidal microcrystalline cellulose to be tested in the mixed solution is 1%; (3) taking the mixed solution obtained in step (2) to centrifuge, drying the obtained precipitate and weighing, and calculating the centrifugal precipitation rate; (4) adding the mixed solution obtained in step (2) into a sealed container and then performing oil bath treatment, stopping the oil bath when one or more non-uniform states of stratification, water separation, agglomeration, flocculation and particle wall hanging appear, and recording the time of the oil bath as the oil bath tolerance time; (5) naturally cooling the mixed solution after the oil bath treatment and pouring, and scoring the pouring state to obtain a pouring score, and when the pouring is smooth and stable, the pouring score is excellent when the water flow diameter is uniform; (6) evaluating by the dry powder particle size, the centrifugal precipitation rate, the oil bath tolerance time and the pouring score; when the dry powder particle size of the colloidal microcrystalline cellulose to be tested is 55 μm≤D[4,3]≤70 μm and d(0.9)≤150 μm, the centrifugal precipitation rate is ≤10%, the oil bath tolerance time is ≥40 min and the pouring score is excellent, the colloidal microcrystalline cellulose to be tested has good suspension performance and processing tolerance and is not easy to form a weak gel by self-aggregation.

2. The method for rapidly evaluating the application performance of colloidal grade microcrystalline cellulose in neutral milk beverage according to claim 1, characterized in that, The temperature of the water in step (2) is normal temperature.

3. A method for rapidly evaluating the performance of colloidal grade microcrystalline cellulose in a neutral milk beverage according to claim 1 or 2, characterized in that, The shearing condition in step (2) is 2500-3000 rpm, the shearing time is 20-30 min, the homogenization pressure of the first stage is 200-300 bar, and the homogenization pressure of the second stage is 40-60 bar.

4. The method for rapidly evaluating the application performance of colloidal grade microcrystalline cellulose in neutral milk beverage according to claim 2, characterized in that, The centrifugal condition in step (3) is 4000-5000 rpm and 20-30 min, and the drying condition is 40-60 °C and 6-12 h.

5. A method for rapidly evaluating the performance of colloidal grade microcrystalline cellulose in a neutral milk beverage according to claim 4, characterized by, The centrifugal precipitation rate (%) in step (3) is (m2-m1) / m×100, wherein m1 is the weight of the centrifugal tube, m is the mass of the mixed solution in the centrifugal tube, and m2 is the mass of the precipitate after drying.

6. The method for rapidly evaluating the application performance of colloidal grade microcrystalline cellulose in neutral milk beverage according to claim 2, characterized in that, The oil bath temperature in step (4) is 130 °C.

7. The method for rapidly evaluating the application performance of colloidal grade microcrystalline cellulose in neutral milk beverage according to claim 2, characterized in that, In step (4), 50-60 g of the mixed solution obtained in step (2) is added into a 100 mL pressure-resistant and heat-resistant bottle, the pressure-resistant and heat-resistant bottle is sealed, heated in an oil bath at 130 °C, and the oil bath is stopped when one or more non-uniform states of stratification, water separation, agglomeration, flocculation and particle wall hanging appear, and the time of the oil bath is recorded as the oil bath tolerance time; the tolerance pressure of the pressure-resistant and heat-resistant bottle is 5-6 bar, and the tolerance temperature is 140-180 °C.

8. The method for rapidly evaluating the application performance of colloidal grade microcrystalline cellulose in neutral milk beverage according to claim 6, characterized in that, In step (5), the natural cooling is air cooling under room temperature in a static state; and the pouring flow rate is 0.05-0.08 m / s.

9. A method for rapidly evaluating the performance of colloidal grade microcrystalline cellulose in neutral milk beverages according to claim 1 or 2 or 5 or 6 or 7 or 8, characterized in that, In step (5), the pouring score standard is: when the stable pouring forms a non-uniform water flow diameter and obvious weak gel appears, the pouring score is poor.

10. A method for rapidly evaluating the performance of colloidal grade microcrystalline cellulose in a neutral milk beverage according to claim 9, characterized by, The evaluation standard of step (6) is: when the dry powder particle size of the colloidal microcrystalline cellulose to be tested is D[4,3]<55 μm and the oil bath tolerance time is <40 min, the colloidal microcrystalline cellulose to be tested has poor processing tolerance. When the particle size D[4,3] of the colloidal microcrystalline cellulose to be measured is greater than 70 μm and the centrifugal precipitation rate is greater than 10%, the colloidal microcrystalline cellulose has poor suspensibility; When the colloidal microcrystalline cellulose to be measured has a poor pouring score, the colloidal microcrystalline cellulose to be measured is prone to self-aggregation and has strong weak gel performance.

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