Preparation method of nanoscale curcumin suspension, curcumin suspension and application

Abstract

The invention relates to the field of medicines and functional foods, in particular to a preparation method of a nanoscale curcumin suspension, the curcumin suspension and application. The preparation method of the nanoscale curcumin suspension comprises the following steps: (1) adding phospholipid and polyglycerol ester into warm water, and carrying out high-speed shearing and uniform dispersion to obtain a mixed solution A; (2) weighing curcumin, adding the curcumin into the mixed solution A, and performing high-speed shearing and uniform dispersion to obtain a mixed solution B; and (3) grinding the mixed solution B in a sand mill to obtain the curcumin suspension, wherein the particle size of the curcumin is 100-200 nm. The curcumin prepared by the preparation method of the curcumin suspension has the characteristics of high loading capacity, high stability and high safety, and solves the problems that in the prior art, the curcumin is low in loading capacity and poor in safety, dissolving equipment is needed during use, and processing aids such as organic solvents are used during processing; the application range of the curcumin is greatly expanded; the preparation convenience is improved.

Description

TECHNICAL FIELD

[0001] The application relates to the fields of medicine and functional food, and particularly relates to a preparation method of nanoscale curcumin suspension, curcumin suspension and application. BACKGROUND

[0002] Curcumin is a low-molecular-weight polyphenol compound extracted from the rhizomes of Curcuma longa, Curcuma wenyujin and Curcuma zedoary, and has physiological activities such as anti-tumor, anti-inflammatory, antioxidant, hypolipidemic, antiviral and anti-atherosclerotic activities. In addition, curcumin is natural, low-toxic and has few adverse reactions, and has excellent coloring ability, and is widely used in the fields of food, medicine and cosmetics. However, curcumin has poor water solubility and poor stability in light, heat and oxygen environment, which leads to low bioavailability, and therefore seriously limits its popularization and utilization.

[0003] In order to improve the water solubility of curcumin and fully utilize its biological activity, some studies are devoted to the preparation of curcumin microemulsion. However, the preparation of microemulsion requires the use of a large amount of surfactant, and the amount of surfactant (such as Tween and sucrose ester) allowed to be added in food is usually strictly limited by regulations (such as the European Union stipulates that the amount of some surfactants added is ≤0.5%), which is far lower than the required concentration of microemulsion. It is difficult to achieve the purpose of effective application in food.

[0004] In addition, the preparation of curcumin microcapsules or nanocapsules by embedding technology is also an important means to improve the stability of curcumin. However, due to the influence of the use environment on the stability of the wall material, curcumin is easy to precipitate after rehydration and dilution. In addition, the current preparation method and product of nanocapsule of curcumin have the problems of unreasonable preparation process, low utilization rate of curcumin as raw material, poor stability of effective ingredient curcumin in product and easy crystallization of oil, etc. The encapsulating material is not appropriate, which leads to poor dissolution or degradation performance in the digestive tract, so that curcumin cannot be released in time, thereby affecting its absorption and utilization.

[0005] There are also studies on the preparation of water-soluble curcumin powder by emulsification technology or the preparation of curcumin suspension by reducing the particle size of curcumin to improve the water solubility of curcumin. However, there are problems such as low loading of effective ingredient curcumin, the need to use additional oil or organic solvent as a processing aid, etc. Therefore, the application of curcumin in the food and pharmaceutical industries is limited. In addition, the powder needs mixing equipment for dissolution, the basic particle size of the existing nanosuspension is large, and the product is unstable and easy to aggregate into larger particles during storage.

[0006] Therefore, at present, the technical problems of simple preparation, convenient use, high safety, high loading and good stability of curcumin have not been fundamentally solved.

[0007] CONTENT OF THE APPLICATION

[0008] To solve the above technical problems, the application provides a preparation method of nanoscale curcumin suspension, the curcumin suspension and application. The preparation method mixes curcumin and a small amount of emulsifier with food safety, and uses a sand mill grinding technique under the process parameters to prepare nanoscale curcumin suspension with high curcumin loading, a particle size of 100-200 nm, high stability and good human safety.

[0009] The object of the application is achieved by the following technical solutions.

[0010] In one aspect, the application provides a preparation method of nanoscale curcumin suspension, comprising the following steps:

[0011] (1) adding phospholipid and polyglycerol ester to warm water, and uniformly dispersing and shearing at high speed to obtain a mixed solution A;

[0012] (2) weighing curcumin and adding it to the mixed solution A, and uniformly dispersing and shearing at high speed to obtain a mixed solution B;

[0013] (3) placing the mixed solution B in a sand mill to grind to obtain the curcumin suspension, wherein the particle size of the curcumin is 100-200 nm.

[0014] For the first aspect of the application, in some specific embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (0.5-3):(0.5-3):(74-86):(12-20).

[0015] For the first aspect of the application, in some specific embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (0.5-3):(0.5-3):(74-86):(12-20).

[0016] For the first aspect of the application, in some specific embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (1-3):(1-3):(74-86):(12-20).

[0017] In some embodiments of the first aspect of the present application, the preparation method comprises the following components in parts by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of polyglycerol ester; specifically, the parts of water can be 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, or any value between any two of the aforementioned values; the parts of curcumin can be 12, 13, 14, 15, 16, 17, 18, 19, 20, or any value between any two of the aforementioned values; the parts of phospholipid can be 0.5, 1, 1.5, 2, 2.5, 3, or any value between any two of the aforementioned values; and the parts of polyglycerol ester can be 0.5, 1, 1.5, 2, 2.5, 3, or any value between any two of the aforementioned values.

[0018] In some embodiments of the first aspect of the present application, the preparation method comprises the following components in parts by weight: 86 parts of water, 12 parts of curcumin, 1 part of phospholipid, and 1 part of polyglycerol ester.

[0019] In some embodiments of the first aspect of the present application, the preparation method comprises the following components in parts by weight: 74 parts of water, 20 parts of curcumin, 3 parts of phospholipid, and 3 parts of polyglycerol ester.

[0020] In some embodiments of the first aspect of the present application, the polyglycerol ester is at least one of hexa-polyglycerol ester, deca-polyglycerol ester, and penta-deca-polyglycerol ester.

[0021] In some embodiments of the first aspect of the present application, the glycerol ester is hexa-polyglycerol ester, and the nano-sized curcumin suspension comprises the following components in parts by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of hexa-polyglycerol ester.

[0022] In some embodiments of the first aspect of the present application, the glycerol ester is deca-polyglycerol ester, and the nano-sized curcumin suspension comprises the following components in parts by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of deca-polyglycerol ester.

[0023] In some embodiments of the first aspect of the present application, the glycerol ester is penta-deca-polyglycerol ester, and the nano-sized curcumin suspension comprises the following components in parts by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of penta-deca-polyglycerol ester.

[0024] For the first aspect of the present application, in some embodiments, the glyceride is a mixture of hexaglycerin ester and pentadecaglycerin fatty acid ester, and the nanoscale curcumin suspension comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, 0.5-1.5 parts of hexaglycerin fatty acid ester, and 0.5-1.5 parts of pentadecaglycerin fatty acid ester.

[0025] For the first aspect of the present application, in some embodiments, the high-speed shearing in step (1) comprises shearing at 2500 rpm-3500 rpm for 5 min-10 min. In some more specific embodiments, the high-speed shearing in step (1) can be performed at a speed of 2500 rpm, 2600 rpm, 2700 rpm, 2800 rpm, 2900 rpm, 3000 rpm, 3100 rpm, 3200 rpm, 3300 rpm, 3400 rpm, 3500 rpm, or any value between any two of the foregoing values. In some more specific embodiments, the high-speed shearing in step (1) can be performed for a time period of 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, or any value between any two of the foregoing values.

[0026] For the first aspect of the present application, in some embodiments, the water temperature of the warm water in step (1) is 68℃-75℃. In some more specific embodiments, the water temperature of the warm water can be 68℃, 69℃, 70℃, 71℃, 72℃, 73℃, 74℃, 75℃, or any value between any two of the foregoing values.

[0027] In some embodiments of the first aspect of the present application, the high-speed shearing in step (2) is performed at 3500 rpm to 6000 rpm for 10 min to 15 min. In some more specific embodiments, the high-speed shearing in step (2) is performed at a speed of 3500 rpm, 3600 rpm, 3700 rpm, 3800 rpm, 3900 rpm, 4000 rpm, 4100 rpm, 4200 rpm, 4300 rpm, 4400 rpm, 4500 rpm, 4600 rpm, 4700 rpm, 4800 rpm, 4900 rpm, 5000 rpm, 5100 rpm, 5200 rpm, 5300 rpm, 5400 rpm, 5500 rpm, 5600 rpm, 5700 rpm, 5800 rpm, 5900 rpm, 6000 rpm, or any value between any two of the aforementioned values. In some more specific embodiments, the high-speed shearing in step (2) is performed for a time period of 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, or any value between any two of the aforementioned values.

[0028] In some embodiments of the first aspect of the present application, the grinding medium of the sand mill in step (3) is zirconium beads, and the particle size of the zirconium beads is 0.2 mm to 0.5 mm, and the rotation speed of the sand mill is 2000 rpm to 2500 rpm. In some more specific embodiments, the particle size of the zirconium beads in step (3) is 0.2 mm, 0.25 mm, 0.3 mm, 0.35 mm, 0.4 mm, 0.45 mm, 0.5 mm, or any value between any two of the aforementioned values. In some more specific embodiments, the rotation speed of the sand mill in step (3) is 2000 rpm, 2100 rpm, 2200 rpm, 2300 rpm, 2400 rpm, 2500 rpm, or any value between any two of the aforementioned values.

[0029] In some embodiments of the first aspect of the present application, the grinding time is 10 min to 30 min.

[0030] In some embodiments of the first aspect of the present application, the method for preparing the nanoscale curcumin suspension comprises the following steps: (1) adding 1 to 3 parts by weight of phospholipid and 1 to 3 parts by weight of polyglycerol ester into 74 to 86 parts of warm water, and uniformly dispersing the mixture by high-speed shearing to obtain a mixed solution A;

[0031] (2) weighing 12 to 20 parts of curcumin, and adding the curcumin into the mixed solution A, and uniformly dispersing the mixture by high-speed shearing to obtain a mixed solution B;

[0032] (3) the mixed solution B is placed in a sand mill to be ground to obtain the curcumin suspension agent, and the particle size of the curcumin is 100 nm to 200 nm; in some embodiments, the particle size of the curcumin can be 100 nm, 105 nm, 110 nm, 115 nm, 120 nm, 125 nm, 130 nm, 135 nm, 140 nm, 145 nm, 150 nm, 155 nm, 160 nm, 165 nm, 170 nm, 175 nm, 180 nm, 185 nm, 190 nm, 195 nm, 200 nm, and any value between any two of the foregoing; in some more specific embodiments, the particle size of the curcumin can be 126.3 nm, 106.7 nm, 116.7 nm, 182.9 nm, respectively.

[0033] The preparation method of the present application can prepare a curcumin suspension agent with small particle size without adding other substances, only containing phospholipids, polyglycerol esters, water and curcumin. The preparation method of the present application can fully utilize phospholipids and polyglycerol esters to fully disperse curcumin, thereby realizing the preparation of a curcumin suspension agent with high loading and small particle size with few additives.

[0034] In a second aspect, the present application provides a nanoscale curcumin suspension agent prepared by the preparation method of any one of claims 1-7.

[0035] Unlike existing curcumin nanosuspensions, the nanoscale curcumin suspension agent of the present application has the characteristics of high loading, high stability and high safety, with a particle size of not more than 200 nm, stable particle size and no aggregation during the entire storage period, high stability, and can greatly improve the bioavailability. Moreover, the suspension agent of the present application has a high curcumin loading, which is a high curcumin suspension agent that cannot be achieved by the current technology with so few other excipients, greatly expanding the application range of curcumin as a food, medicine and cosmetic raw material. In addition, the preparation process of the present application only uses a small amount of food-grade emulsifier, which has high safety and can be used as a raw material and coloring agent with peace of mind. Finally, the present application is simple to operate and can be realized by simply mixing the materials and grinding them in a sand mill, which has strong promotional value.

[0036] In some specific embodiments of the second aspect of the present application, the nanoscale curcumin suspension agent is composed of phospholipids, polyglycerol esters, water and curcumin.

[0037] In some specific embodiments of the second aspect of the present application, the nanoscale curcumin suspension agent is composed of phospholipids, polyglycerol esters, water and curcumin; and the weight ratio of the phospholipids, polyglycerol esters, warm water and curcumin is (1-3) :(1-3) :(74-86) :(12-20).

[0038] The particle size distribution of the product is a main factor affecting the settling of particulate matter. Normally, the settling speed of particulate matter is proportional to the particle size thereof. The smaller the particle size and the more uniform the distribution, the slower the settling speed, and the better the stability of the product. Therefore, the curcumin suspension prepared in the present application has small particle size and good stability.

[0039] For the second aspect of the present application, the nanoscale curcumin suspension can contain only phospholipid, polyglycerol ester, warm water and curcumin, or can contain other reagents commonly used for preparing curcumin suspension. However, compared with the prior art which uses a large amount of various reagents to prepare curcumin suspension, the present application can produce a curcumin suspension with high safety to human body, higher loading, smaller particle size, containing only phospholipid, polyglycerol ester, warm water and curcumin.

[0040] The third aspect of the present application provides an application of the nanoscale curcumin suspension prepared by the preparation method of any one of the first aspect in the field of medicine or food.

[0041] Compared with the prior art, the present application has the following technical effects:

[0042] (1) The nanoscale curcumin suspension prepared in the present application has high loading, high stability and high safety, and solves the problems of low curcumin loading, poor safety, the need for dissolution equipment during use, and the use of organic solvents and other processing aids during processing in the prior art, greatly expanding the application range of curcumin.

[0043] (2) The nanoscale curcumin suspension prepared in the present application uses a small amount of food-grade surfactant as a suspending agent to disperse curcumin particles in water, and forms a stable nanocolloidal dispersion through grinding technology. It has high dispersion degree and good consistency, is beneficial to the dissolution and absorption of drugs, and can greatly improve the bioavailability of drugs.

[0044] (3) The nanoscale curcumin suspension prepared in the present application will not aggregate and precipitate during storage, and as a raw material, there is no quality problem and quality risk.

[0045] (4) The present application is simple to operate and can be realized by simply mixing materials and grinding with a sand mill, and has strong popularization value. BRIEF DESCRIPTION OF DRAWINGS

[0046] Figure 1 The particle size distribution graph of Example 1 of the present application;

[0047] Figure 2 The stability analysis graph of Example 1 of the present application;

[0048] Figure 3Particle size distribution chart of the comparative example 1, the comparative example 2 and the comparative example 3 of the present application;

[0049] Figure 4 Stability analysis chart of the comparative example 1 of the present application;

[0050] Figure 5 Stability analysis chart of the comparative example 2 of the present application;

[0051] Figure 6 Stability analysis chart of the comparative example 3 of the present application. DETAILED DESCRIPTION

[0052] The technical solutions of the present application are further specifically described below through specific examples, but the protection scope of the present application is not limited thereto.

[0053] In the present application, the raw materials and equipment used are commercially available or common in the art, unless otherwise specified. The methods in the following examples are conventional methods in the art, unless otherwise specified.

[0054] Raw materials:

[0055] Curcumin is provided by Aikaiwei (Beijing) Trade Co., Ltd., with a purity of 95%;

[0056] Phospholipids are provided by Cargill Investment (China) Co., Ltd., with an acetone insoluble content of ≥95%;

[0057] Polyglycerol esters are provided by Shandong Binzhou Jinsheng New Material Technology Co., Ltd., with an effective content of >98%;

[0058] Detection method:

[0059] Lumisizer stability analyzer is used for stability determination

[0060] Lumisizer stability analyzer is a technical solution for accelerating the evaluation of the sedimentation of samples in the shelf life by centrifugal force, and deducing whether the system is stable, by centrifugal force to make each component in the beverage float or precipitate under the action of gravity or centrifugal force, and then use light source to irradiate to get real-time monitoring transmittance spectrum.

[0061] In the present application, Lumisizer stability analyzer is used to detect the stability of curcumin suspensions obtained in each example and comparative example, and the test conditions are: 500 spectrum lines are tested at 25℃, 4000rpm / min for 5s per bar.

[0062] Particle size determination

[0063] The particle size of the curcumin suspensions obtained in each example and comparative example was detected by a Malvern Mastersizer 3000 laser particle size analyzer. The test conditions were: 25℃, 1800rpm / min.

[0064] In one aspect, the present application provides a preparation method of a nano-scale curcumin suspension, comprising the following steps:

[0065] (1) phospholipid and polyglycerol ester were added into warm water, and high-speed shearing was performed to uniformly disperse to obtain a mixed solution A;

[0066] (2) curcumin was weighed and added into the mixed solution A, and high-speed shearing was performed to uniformly disperse to obtain a mixed solution B;

[0067] (3) the mixed solution B was placed in a sand mill for grinding to obtain the curcumin suspension, and the particle size of the curcumin was 100nm-200nm.

[0068] For the first aspect of the present application, in some embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (0.5-3):(0.5-3):(74-86):(12-20).

[0069] For the first aspect of the present application, in some embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (0.5-3):(0.5-3):(74-86):(12-20).

[0070] For the first aspect of the present application, in some embodiments, the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (1-3):(1-3):(74-86):(12-20).

[0071] For the first aspect of the present application, in some embodiments, the preparation method comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of polyglycerol ester. Specifically, the number of parts of the water can be 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, or any value between any two of the foregoing values. The number of parts of the curcumin can be 12, 13, 14, 15, 16, 17, 18, 19, 20, or any value between any two of the foregoing values. The number of parts of the phospholipid can be 0.5, 1, 1.5, 2, 2.5, 3, or any value between any two of the foregoing values. The number of parts of the polyglycerol ester can be 0.5, 1, 1.5, 2, 2.5, 3, or any value between any two of the foregoing values.

[0072] For the first aspect in the embodiments of the present application, in some embodiments, the preparation method comprises the following components by weight: 86 parts of water, 12 parts of curcumin, 1 part of phospholipid, and 1 part of polyglycerol ester.

[0073] For the first aspect in the embodiments of the present application, in some embodiments, the preparation method comprises the following components by weight: 74 parts of water, 20 parts of curcumin, 3 parts of phospholipid, and 3 parts of polyglycerol ester.

[0074] For the first aspect in the embodiments of the present application, in some embodiments, the polyglycerol ester is at least one of hexaglycerol ester, decaglycerol fatty acid ester, and pentadecaglycerol fatty acid ester.

[0075] For the first aspect in the embodiments of the present application, in some embodiments, the glycerol ester is hexaglycerol fatty acid ester, and the nanoscale curcumin suspension comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of hexaglycerol fatty acid ester.

[0076] For the first aspect in the embodiments of the present application, in some embodiments, the glycerol ester is decaglycerol fatty acid ester, and the nanoscale curcumin suspension comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of decaglycerol fatty acid ester.

[0077] For the first aspect in the embodiments of the present application, in some embodiments, the glycerol ester is pentadecaglycerol fatty acid ester, and the nanoscale curcumin suspension comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, and 1-3 parts of pentadecaglycerol fatty acid ester.

[0078] For the first aspect in the embodiments of the present application, in some embodiments, the glycerol ester is a mixture of hexaglycerol ester and pentadecaglycerol fatty acid ester, and the nanoscale curcumin suspension comprises the following components by weight: 74-86 parts of water, 12-20 parts of curcumin, 1-3 parts of phospholipid, 0.5-1.5 parts of hexaglycerol fatty acid ester, and 0.5-1.5 parts of pentadecaglycerol fatty acid ester.

[0079] For the first aspect in the embodiments of the present application, in some embodiments, the high-speed shearing in step (1) comprises shearing at 2500 rpm to 3500 rpm for 5 min to 10 min; in some more specific embodiments, the high-speed shearing in step (1) can be at a speed of 2500 rpm, 2600 rpm, 2700 rpm, 2800 rpm, 2900 rpm, 3000 rpm, 3100 rpm, 3200 rpm, 3300 rpm, 3400 rpm, 3500 rpm, or any value between any two of the foregoing values; in some more specific embodiments, the high-speed shearing in step (1) can be for a time period of 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, or any value between any two of the foregoing values.

[0080] For the first aspect in the embodiments of the present application, in some embodiments, the water temperature of the warm water in step (1) is 68℃ to 75℃; in some more specific embodiments, the water temperature of the warm water can be 68℃, 69℃, 70℃, 71℃, 72℃, 73℃, 74℃, 75℃, or any value between any two of the foregoing values.

[0081] For the first aspect in the embodiments of the present application, in some embodiments, the high-speed shearing in step (2) comprises shearing at 3500 rpm to 6000 rpm for 10 min to 15 min; in some more specific embodiments, the high-speed shearing in step (2) can be at a speed of 3500 rpm, 3600 rpm, 3700 rpm, 3800 rpm, 3900 rpm, 4000 rpm, 4100 rpm, 4200 rpm, 4300 rpm, 4400 rpm, 4500 rpm, 4600 rpm, 4700 rpm, 4800 rpm, 4900 rpm, 5000 rpm, 5100 rpm, 5200 rpm, 5300 rpm, 5400 rpm, 5500 rpm, 5600 rpm, 5700 rpm, 5800 rpm, 5900 rpm, 6000 rpm, or any value between any two of the foregoing values; in some more specific embodiments, the high-speed shearing in step (2) can be for a time period of 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, or any value between any two of the foregoing values.

[0082] For the first aspect in the specific embodiments of the present application, in some embodiments, the grinding medium of the sand mill in step (3) is zirconium beads; the particle size of the zirconium beads is 0.2mm-0.5mm, and the rotation speed of the sand mill is 2000rpm-2500rpm; in some more specific embodiments, the particle size of the zirconium beads in step (3) can be 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm, 0.5mm, and any value between any two of the foregoing values; in some more specific embodiments, the rotation speed of the sand mill in step (3) can be 2000rpm, 2100rpm, 2200rpm, 2300rpm, 2400rpm, 2500rpm, and any value between any two of the foregoing values.

[0083] For the first aspect in the specific embodiments of the present application, in some embodiments, the grinding time is 10min-30min.

[0084] For the first aspect in the specific embodiments of the present application, in some embodiments, the preparation method of the nanoscale curcumin suspension comprises: (1) adding 1-3 parts by weight of phospholipid and 1-3 parts by weight of polyglycerol ester into 74-86 parts of warm water, and uniformly dispersing by high-speed shearing to obtain a mixed solution A;

[0085] (2) weighing 12-20 parts of curcumin and adding it into the mixed solution A, and uniformly dispersing by high-speed shearing to obtain a mixed solution B;

[0086] (3) placing the mixed solution B in a sand mill for grinding to obtain the curcumin suspension, wherein the particle size of the curcumin is 100nm-200nm; in some embodiments, the particle size of the curcumin can be 100nm, 105nm, 110nm, 115nm, 120nm, 125nm, 130nm, 135nm, 140nm, 145nm, 150nm, 155nm, 160nm, 165nm, 170nm, 175nm, 180nm, 185nm, 190nm, 195nm, 200nm, and any value between any two of the foregoing values; in some more specific embodiments, the particle size of the curcumin can be 126.3nm, 106.7nm, 116.7nm, 182.9nm, respectively.

[0087] The preparation method of the present application can prepare a curcumin suspension with small particle size without adding other substances, only containing phospholipid, polyglycerol ester, water, and curcumin. The preparation method of the present application can fully utilize phospholipid and polyglycerol ester to fully disperse curcumin, and achieve the preparation of a curcumin suspension with high loading and small particle size with few additives.

[0088] In a second aspect, the embodiments of the present application provide a nanoscale curcumin suspension prepared by the preparation method of any one of claims 1-7.

[0089] Unlike the existing nanoscale curcumin suspension, the nanoscale curcumin suspension of the present application has the characteristics of high loading, high stability and high safety, the particle size is not greater than 200 nm, the particle size is stable and does not aggregate during the entire storage period, has high stability, and can greatly improve the bioavailability. Moreover, the suspension of the present application has a high curcumin loading, which is a high loading curcumin suspension that cannot be achieved by the current technology using such a small amount of other auxiliary materials, greatly expanding the application range of curcumin as a food, medicine and cosmetic raw material. In addition, the preparation process of the present application only uses a small amount of food-grade emulsifier, which has high safety and can be used as a raw material and coloring agent with peace of mind. Finally, the present application is simple to operate and can be realized by simply mixing the materials and grinding them in a sand mill, which has strong promotional value.

[0090] For the second aspect of the embodiments of the present application, in some embodiments, the nanoscale curcumin suspension is composed of phospholipid, polyglycerol ester, water and curcumin.

[0091] For the second aspect of the embodiments of the present application, in some embodiments, the nanoscale curcumin suspension is composed of phospholipid, polyglycerol ester, water and curcumin; and the weight ratio of the phospholipid, polyglycerol ester, warm water and curcumin is (1-3) :(1-3) :(74-86) :(12-20).

[0092] The particle size distribution of the product is a major factor affecting the settling of particulate matter. Under normal circumstances, the settling speed of particulate matter is proportional to its particle size, the smaller the particle size and the more uniform the distribution, the slower the settling speed, and the better the stability of the product. Therefore, the curcumin suspension prepared by the present application has small particle size and good stability.

[0093] For the second aspect of the embodiments of the present application, the nanoscale curcumin suspension can contain only phospholipid, polyglycerol ester, warm water and curcumin, or can contain other reagents commonly used for preparing curcumin suspension. However, compared with the prior art which uses a large amount of multiple reagents to prepare curcumin suspension, the present application can produce a curcumin suspension containing only phospholipid, polyglycerol ester, warm water and curcumin, which has high safety and higher loading and smaller particle size.

[0094] The third aspect of the embodiments of the present application provides the use of the nanoscale curcumin suspension prepared by the preparation method of any one of the first aspect in the field of medicine or food.

[0095] Example 1:

[0096] (1) 1 part by weight of phospholipid and 1 part by weight of polyglycerol ester were added to 86 parts of warm water at 68°C, and dispersed uniformly at 2500 rpm for 5 min to obtain a mixed solution A;

[0097] (2) 12 parts of curcumin were weighed and added to the mixed solution A, and dispersed uniformly at 2500 rpm for 10 min to obtain a mixed solution B;

[0098] (3) The mixed solution B was placed in a sand mill, and 0.2 mm size zirconium beads were selected for grinding at 2000 rpm to obtain a nano-sized curcumin suspension preparation 1. The particle size and stability of the nano-sized curcumin suspension preparation 1 were analyzed according to the above detection method, as shown in Figure 1 , the particle size distribution of the nano-sized curcumin suspension preparation 1, and the (average) particle size measured was 126.3 nm; Figure 1 Figure 2 was the stability analysis of the nano-sized curcumin suspension preparation 1, wherein Figure 2 the X-axis represents the sample tube length in millimeters / mm, representing the position of the sample in the detection tube; the Y-axis represents the transmission rate (%), reflecting the sample concentration distribution, and the higher the transmission rate, the lower the particle / drop concentration in this area (such as the supernatant). It can be seen from Figure 2 that the transmission rate at the top and bottom of the curcumin suspension liquid did not change significantly under the action of centrifugal force over time, indicating that the suspension liquid has good stability.

[0099] The curcumin loading in this example was 12%.

[0100] Example 2:

[0101] (1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 68°C, and dispersed uniformly at 2500 rpm for 5 min to obtain a mixed solution A;

[0102] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and dispersed uniformly at 2500 rpm for 10 min to obtain a mixed solution B;

[0103] (3) The mixed solution B was placed in a sand mill, and 0.2 mm size zirconium beads were selected for grinding at 2000 rpm to obtain a nano-sized curcumin suspension preparation 2. The (average) particle size of the nano-sized curcumin suspension preparation 2 was 106.7 nm, and the loading was 20%.

[0104] Example 3:

[0105] ​(1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 75°C, and dispersed uniformly at 3500 rpm for 10 min to obtain a mixed solution A;

[0106] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and dispersed uniformly at 6000 rpm for 15 min to obtain a mixed solution B;

[0107] (3) The mixed solution B was placed in a sand mill, and zirconium beads with a size of 0.2 mm were selected for grinding at 2000 rpm to obtain a nano curcumin suspension preparation 3, which had an average particle size of 116.7 nm and a loading of 20%.

[0108] Example 4:

[0109] (1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 68°C, and dispersed uniformly at 2500 rpm for 5 min to obtain a mixed solution A;

[0110] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and dispersed uniformly at 2500 rpm for 10 min to obtain a mixed solution B;

[0111] (3) The mixed solution B was placed in a sand mill, and zirconium beads with a size of 0.5 mm were selected for grinding at 2500 rpm to obtain a nano curcumin suspension preparation 4, which had an average particle size of 182.9 nm and a loading of 20%.

[0112] Comparative Example 1

[0113] The difference between this comparative example and Example 2 is that the phospholipid and polyglycerol ester were mixed without shearing and directly mixed with curcumin, and the sheared product was not ball milled, and other conditions were the same. The specific steps are as follows:

[0114] (1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 68°C to obtain a mixed solution A;

[0115] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and dispersed uniformly at 2500 rpm for 10 min to obtain a mixed solution B; and a curcumin suspension preparation 5 was obtained.

[0116] In the above preparation method, the solution obtained by mixing the phospholipid and polyglycerol ester without shearing and directly mixing with curcumin was separated into layers; the particle size of the curcumin suspension 5 obtained by the above method was greater than 200 nm, and the particle size distribution was shown in the spectrum as described in Figure 1# of Table 1, and specifically shown in the detection data of the sample 1# in Table 1. The stability spectrum is shown in Figure 3 Figure 4 ​​

[0117] Comparative Example 2

[0118] The difference between this comparative example and Example 2 is that steps (1) and (2) are the same, and there is no step (3). The specific steps are as follows:

[0119] (1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 68°C, and high-speed shearing at 2500 rpm for 5 min to disperse uniformly to obtain a mixed solution A;

[0120] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and high-speed shearing at 2500 rpm for 10 min to disperse uniformly to obtain a mixed solution B; curcumin suspension preparation 6 was obtained.

[0121] In the above preparation method, the phospholipid and polyglycerol ester mixture and the solution obtained by directly mixing with curcumin without shearing were separated into layers; the particle size of the curcumin suspension 5 obtained by the above method was greater than 200 nm, and the particle size distribution was as shown in the graph described in Table 2#. Figure 3 The detection data of sample 2# in Table 2 are shown in detail. The stability graph is shown in Figure 5 .

[0122] Comparative Example 3

[0123] The difference between this comparative example and Example 2 is that steps (1) and (2) are the same, and there is no step (3). The specific steps are as follows: steps (1) and (2) are the same, and step (3) is high-pressure homogenization. The specific steps are as follows.

[0124] (1) 3 parts by weight of phospholipid and 3 parts by weight of polyglycerol ester were added to 74 parts of warm water at 68°C, and high-speed shearing at 2500 rpm for 5 min to disperse uniformly to obtain a mixed solution A;

[0125] (2) 20 parts of curcumin were weighed and added to the mixed solution A, and high-speed shearing at 2500 rpm for 10 min to disperse uniformly to obtain a mixed solution B;

[0126] (3) The mixed solution B was placed in a high-pressure homogenizer, and homogenized 10 times at a pressure of 20000 psi to obtain curcumin suspension preparation 7.

[0127] In the above preparation method, on the one hand, the hard particles seriously wear the homogenizer head, and on the other hand, the particle size of the curcumin obtained by this method is still greater than 200 nm; the particle size distribution is as shown in the graph described in Table 3#. Figure 3 The detection data of sample 3# in Table 1 are shown in detail. The stability graph is shown in Figure 6 . Figure 6It can be seen that the top transmittance of the curcumin suspension gradually increases with the lapse of time under the action of centrifugal force, which indicates that the particles gradually sink under the action of centrifugal force, so that the particle concentration at the top of the sample decreases, thereby increasing the transmittance; at the same time, the downward migration of the particles leads to the decrease of the bottom transmittance. From the above information, it can be seen that the stability of the curcumin suspension is poor, and there will be unevenness between the top and bottom during the storage period.

[0128] Table 1

[0129] Sample Name d(0.1) d(0.5) d(0.9) D[4,3] 1#3.30 0.354 0.813 1.357 0.844 2#3.30 0.26 0.648 1.318 0.728 3#3.30 0.21 0.419 0.99 0.521

[0130] The above are only preferred embodiments of the present application, and do not limit the patent scope of the present application, and any equivalent structure or equivalent process transformation made by using the specification of the present application, or directly or indirectly used in other related technical fields, are also included in the patent protection scope of the present application.

Claims

1. A method for preparing a nano-sized curcumin suspension, characterized in that, Includes the following steps: (1) Add phospholipids and polyglycerol esters to warm water and disperse them evenly by high-speed shearing to obtain mixture A; (2) Weigh out curcumin and add it to mixture A, then disperse it evenly by high-speed shearing to obtain mixture B; (3) The mixture B is placed in a sand mill and ground to obtain the curcumin suspension, wherein the curcumin particle size is 100nm~200nm.

2. The preparation method according to claim 1, characterized in that, The weight ratio of the phospholipid, polyglycerol ester, warm water, and curcumin is (0.5-3):(0.5-3):(74-86):(12-20).

3. The preparation method according to claim 1, characterized in that, The preparation method comprises the following components in parts by weight: 74-86 parts water, 12-20 parts curcumin, 1-3 parts phospholipids, and 1-3 parts polyglycerol esters.

4. The preparation method according to claim 1, characterized in that, The polyglycerol ester is at least one of hexaglycerol ester, decaglycerol fatty acid ester, and pentadecylglycerol fatty acid ester.

5. The preparation method according to any one of claims 1-4, characterized in that, In step (1), the high-speed shearing includes shearing at 2500 rpm to 3500 rpm for 5 min to 10 min; Preferably, in step (1), the water temperature is 68℃~75℃.

6. The preparation method according to any one of claims 1-4, characterized in that, In step (2), the high-speed shearing includes shearing at 3500rpm to 6000rpm for 10min to 15min.

7. The preparation method according to any one of claims 1-4, characterized in that, In step (3), the grinding media of the sand mill is zirconium beads; the particle size of the zirconium beads is 0.2mm to 0.5mm, and the rotation speed of the sand mill is 2000rpm to 2500rpm.

8. A nano-sized curcumin suspension, characterized in that, The nano-sized curcumin suspension was prepared using the preparation method described in any one of claims 1-7.

9. The preparation method according to claim 8, characterized in that, The nano-sized curcumin suspension is composed of phospholipids, polyglycerol esters, water, and curcumin. Preferably, the weight ratio of the phospholipid, polyglycerol ester, warm water, and curcumin is (1-3):(1-3):(74-86):(12-20).

10. The application of a nano-sized curcumin suspension prepared by any one of claims 1-7 in the pharmaceutical or food fields.

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