Preparation method of ultra-micro emulsified liquid calcium for improving utilization rate of calcium, VD and VK

Abstract

The invention discloses a preparation method of ultra-micro emulsified liquid calcium capable of improving the utilization rate of calcium, VD and VK, which comprises the following steps: adding suspended calcium citrate, self-emulsified VD, VK, a suspending aid, an acidulant, a sweetening agent and essence into a water-containing emulsifying pot, uniformly stirring, homogenizing and emulsifying by a high-speed shearing emulsifying machine to obtain primary emulsified liquid, and adding the primary emulsified liquid into a high-speed shearing emulsifying machine to obtain the ultra-micro emulsified liquid calcium. And further treating the primary emulsion by using a high-pressure homogenizer to obtain the ultra-micro emulsified liquid calcium. According to the technical scheme, the stability and the utilization rate of the calcium, the VD and the VK are improved, the irritation of the calcium, the VD and the VK to the stomach is reduced, a more convenient and more comfortable taking mode is provided, and the tablet has greater advantages especially for groups with dysphagia, such as old people, children and people with dysphagia.

Description

Technical Field

[0001] The invention relates to the technical field of nutritional health products, in particular to a method for preparing ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK. Background Art

[0002] In the field of nutritional supplements, calcium, vitamin D and vitamin K (hereinafter referred to as "VD and VK") are important nutrients that play an important role in maintaining human health. Among them, calcium is an important component of bones and teeth, and is also involved in many physiological processes such as blood coagulation, nerve conduction and muscle contraction. VD and VK help absorb and utilize calcium, promote bone health, and participate in the blood coagulation process. Therefore, supplementing calcium, VD and VK is an important means to prevent and treat diseases such as osteoporosis and rickets.

[0003] Although existing technical means can improve the bioavailability of calcium, VD and VK to a certain extent, there are still some significant problems. First, the absorption rate of calcium, VD and VK in the gastrointestinal tract is not high, resulting in unsatisfactory calcium supplementation effect. Studies have shown that the absorption of calcium, VD and VK is affected by many factors, such as gastric acidity, bile salt concentration, food ingredients, etc. Secondly, most of the existing technologies are single emulsification or dissolution technologies, which are difficult to comprehensively improve the bioavailability of the product. For example, although the addition of vitamin C can promote the absorption of calcium, it may affect the stability of VD. Third, under ordinary emulsification technology, liquid calcium DK oral solution is prone to stratification, precipitation and other phenomena during storage and transportation, affecting product quality and effect. Therefore, how to comprehensively utilize a variety of technical means to comprehensively improve the bioavailability and stability of calcium, VD and VK is an important challenge facing current technology. Summary of the invention

[0004] The technical problem to be solved by the present invention is to overcome the defects of the above prior art and provide a method for preparing ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK, so as to solve the problems of low utilization rate of ordinary liquid calcium oral solution and instability such as precipitation during production or storage.

[0005] The technical solution adopted by the present invention to solve the technical problem is: a method for preparing ultrafine emulsified liquid calcium for improving the utilization rate of calcium, VD and VK, comprising the following steps:

[0006] Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add 0.1-2 parts of suspending agent, 0.1-1 parts of acidulant, 5-15 parts of sweetener, 0.1-2 parts of flavor, 60-90 parts of water, start the stirring device, and stir evenly;

[0007] Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed;

[0008] Step 3: using a high-speed shear emulsifier to treat the mixture obtained in step 2, and obtaining a primary emulsion after the treatment;

[0009] Step 4: further treating the primary emulsified liquid with a high-pressure homogenizer for 1 to 5 times to obtain ultrafine emulsified liquid calcium.

[0010] Furthermore, the suspending agent in step one is selected from one or more of xanthan gum and gum arabic, the acidulant is selected from citric acid, and the sweetener is selected from one or more of white sugar, xylitol, steviol glycoside, and fructose.

[0011] Furthermore, the self-emulsifying system includes vitamin D oil, vitamin K oil, emulsifier and co-emulsifier, and the weight proportions are: 20-60 parts of vitamin D oil and vitamin K oil, 30-50 parts of emulsifier, and 0-50 parts of co-emulsifier.

[0012] Furthermore, the emulsifier is one or more of Tween 20, Tween 80, polyglycerol ester, phospholipid, and sucrose ester, and the co-emulsifier is one or more of propylene glycol and glycerol.

[0013] Furthermore, in step 1 and step 2, the speed of the stirring device is set to 60 rpm / min.

[0014] Furthermore, in step three, the speed of the high-speed shear emulsifier is set to 5000 rpm / min, and the emulsification time is 30 to 40 min.

[0015] Furthermore, in step 4, the pressure of the high-pressure homogenizer is set to 400-800 bar, and the number of homogenization times is 3 times.

[0016] The method for preparing ultrafine emulsified liquid calcium for improving the utilization rate of calcium, VD and VK of the present invention has the following beneficial effects:

[0017] 1. Improve the utilization rate of calcium: The present invention adopts ultra-microemulsification technology, so that calcium ions can be absorbed more quickly and completely in the body, thereby improving the utilization rate of calcium. Compared with the utilization rate of traditional inorganic calcium carbonate, which is only about 20-30%, the calcium utilization rate of the present invention is significantly improved.

[0018] 2. Enhance the stability and utilization of VD and VK: Vitamin D and vitamin K are easily degraded in traditional calcium supplement products, but the ultrafine emulsification technology of the present invention can effectively protect these vitamins, making them less likely to degrade during storage and digestion, and the utilization of VD and VK after self-emulsification is greatly improved.

[0019] 3. Reduce gastric irritation: Traditional calcium supplement products use inorganic calcium carbonate, which is very irritating to the stomach. However, the oral liquid calcium product of the present invention uses ultra-microemulsification technology, which allows calcium ions to be more evenly dispersed in the liquid, reducing the chance of direct contact with the gastric mucosa, thereby reducing gastric irritation.

[0020] 4. Novel dosage form, easy to take: The oral liquid calcium product of the present invention, unlike traditional tablets, has a novel dosage form and is more convenient to take, especially for groups with swallowing difficulties, such as the elderly, children and people with swallowing difficulties.

[0021] 5. Better comprehensive effect: Since the utilization rate of calcium, vitamin D and vitamin K in the present invention is improved, the comprehensive effect is also better, which can more effectively promote the health of bones and teeth and prevent diseases such as osteoporosis. In general, compared with the prior art, the present invention has significant advantages in improving the stability of calcium and vitamin DK, enhancing the utilization rate of calcium and vitamins, reducing gastric irritation, novel dosage form, convenient administration and better comprehensive effect. DETAILED DESCRIPTION

[0022] The present invention will now be further described in detail with reference to the examples and results.

[0023] In the present invention, unless otherwise specified, all parts and percentages are by weight, and the equipment and raw materials used are commonly used in the art and comply with regulations.

[0024] 1. Example 1

[0025] (1) Preparation method

[0026] Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add xanthan gum, citric acid, white sugar, essence, water, start the stirring device, speed 60rpm / min, stir evenly;

[0027] Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed;

[0028] Step 3: homogenize the mixture obtained in step 2 using a high-speed shear emulsifier at 5000 rpm / min and emulsify for 40 minutes to obtain a primary emulsion after the treatment;

[0029] Step 4: Use a high-pressure homogenizer to perform high-pressure homogenization on the primary emulsion at 400 bar. After two times of treatment, ultrafine emulsified liquid calcium is obtained.

[0030] The formula components are as follows:

[0031] ①Formulation components of self-emulsifying system

[0032] Material Name Weight Percent Vitamin D 21.5％ Vitamin K 21.5％ Twain 80 54％ Glycerol 3％

[0033] ②Ultrasonic emulsified liquid calcium formula components

[0034]

[0035]

[0036] (2) Stability test

[0037] Take 45g of the above liquid calcium sample and place it in a 50ml graduated centrifuge tube. Centrifuge at 3500rpm for 10min. Pour naturally until no sample flows out. Turn the centrifuge tube upside down on a paper towel. Record the mass of the centrifuge tube after 10min. No obvious oil-water separation phenomenon occurs in the sample after centrifugation.

[0038] 2. Example 2

[0039] (1) Preparation method

[0040] Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add xanthan gum, gum arabic, citric acid, xylitol, essence, water, start the stirring device, speed 60rpm / min, stir evenly;

[0041] Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed;

[0042] Step 3: The mixture obtained in step 2 is treated by a high-speed shear emulsifier, homogenized at 5000 rpm / min, and emulsified for 40 minutes to obtain a primary emulsion after the treatment is completed;

[0043] Step 4: Use a high-pressure homogenizer to perform high-pressure homogenization on the primary emulsion at 500 bar. After two times of treatment, ultrafine emulsified liquid calcium is obtained.

[0044] The formula components are as follows:

[0045] ①Formulation components of self-emulsifying system

[0046] Material Name Weight Percent Vitamin D 28％ Vitamin K 28％ Twain 80 1％ Polyglycerol esters 42％ Glycerol 1％

[0047] ②Ultrasonic emulsified liquid calcium formula components

[0048] Material Name Weight Percent Calcium Citrate 15％ Self-emulsifying vitamin DK 0.1％ Xanthan gum 0.5％ Gum Arabic 1％ Citric Acid 0.3％ Xylitol 8％ essence 0.5％ water 74.6％

[0049] (2) Stability test

[0050] Take 45g of the above liquid calcium sample and place it in a 50ml graduated centrifuge tube. Centrifuge at 3500rpm for 10min. Pour naturally until no sample flows out. Turn the centrifuge tube upside down on a paper towel. Record the mass of the centrifuge tube after 10min. No obvious oil-water separation phenomenon occurs in the sample after centrifugation.

[0051] 3. Example 3

[0052] (1) Preparation method

[0053] Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add xanthan gum, gum arabic, citric acid, xylitol, essence, water, start the stirring device, speed 60rpm / min, stir evenly;

[0054] Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed;

[0055] Step 3: The mixture obtained in step 2 is treated by a high-speed shear emulsifier, homogenized at 5000 rpm / min, and emulsified for 35 minutes to obtain a primary emulsion after the treatment is completed;

[0056] Step 4: Use a high-pressure homogenizer to perform high-pressure homogenization on the primary emulsion at 600 bar. After two times of treatment, ultrafine emulsified liquid calcium is obtained.

[0057] The formula components are as follows:

[0058] ①Formulation components of self-emulsifying system

[0059] Material Name Weight Percent Vitamin D 15％ Vitamin K 15％ Twain 80 10％ Phospholipids 12％ Glycerol 48％

[0060] ②Ultrasonic emulsified liquid calcium formula components

[0061] Material Name Weight Percent Calcium Citrate 15％ Self-emulsifying vitamin DK 0.2％ Xanthan gum 0.6％ Gum Arabic 1％ Citric Acid 0.4％ Stevioside 0.02％ essence 0.5％ water 82.28％

[0062] (2) Stability test

[0063] Take 45g of the above liquid calcium sample and place it in a 50ml graduated centrifuge tube. Centrifuge at 3500rpm for 10min. Pour naturally until no sample flows out. Turn the centrifuge tube upside down on a paper towel. Record the mass of the centrifuge tube after 10min. The sample after centrifugation shows slight oil-water separation.

[0064] 4. Example 4

[0065] (1) Preparation method

[0066] Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add xanthan gum, gum arabic, citric acid, xylitol, essence, water, start the stirring device, speed 60rpm / min, stir evenly;

[0067] Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed;

[0068] Step 3: The mixture obtained in step 2 is treated by a high-speed shear emulsifier, homogenized at 5000 rpm / min, and emulsified for 35 minutes to obtain a primary emulsion after the treatment is completed;

[0069] Step 4: Use a high-pressure homogenizer to perform high-pressure homogenization on the primary emulsion at 800 bar. After one treatment, ultrafine emulsified liquid calcium is obtained.

[0070] The formula components are as follows:

[0071] ①Formulation components of self-emulsifying system

[0072] Material Name Weight Percent Vitamin D 15％ Vitamin K 15％ Twain 80 10％ Phospholipids 12％ glycerin 48％

[0073] ②Ultrasonic emulsified liquid calcium formula components

[0074]

[0075]

[0076] (2) Stability test

[0077] Take 45g of the above liquid calcium sample and place it in a 50ml graduated centrifuge tube. Centrifuge at 3500rpm for 10min. Pour naturally until no sample flows out. Turn the centrifuge tube upside down on a paper towel. Record the mass of the centrifuge tube after 10min. The sample after centrifugation shows slight oil-water separation.

[0078] 5. In vitro absorption test

[0079] The in vitro test simulated the gastrointestinal digestive tract to explore the bioavailability of calcium, VD, and VK in the liquid calcium oral liquid products obtained in the above Examples 1-4: the liquid calcium products and calcium tablets without ultramicroemulsification were used as controls, and the contents of calcium, VD, and VK in the controls and liquid calcium products were measured before digestion; 50 mL of pure water was added to 1 g of the control / ultramicroemulsified sample. The pH of the fish oil solution was adjusted to 2.0 with 1M hydrochloric acid and allowed to stand in a shaker at 37°C for 10 min. Then 0.25 mL of gastric juice (0.1M HCl containing 4% pepsin, m / v) was added and digested in a shaker at 150 r / min and 37°C for 2 h. The sample was then centrifuged at 4°C and 8000 r / min for 15 min, the precipitate was discarded, the supernatant was taken, the digestion solution was heated and boiled for 5 min to inactivate the enzyme, and then filtered through a 0.22 μm filter membrane to measure the contents of calcium, VD, and VK in the digestion solution.

[0080] The pH of the pepsin digestion solution was adjusted to 7.0 with saturated NaHCO3, and 1 mL of intestinal fluid (0.01 M PBS containing 1% trypsin, m / v) was added, and then digested for 2 h in a shaker at 150 r / min and 37°C. After digestion, centrifugation, enzyme inactivation, membrane filtration, and determination of calcium, VD, and VK content in the digestion solution were performed.

[0081] The bioavailability of calcium, VD, and VK in fish oil is expressed by the following formula:

[0082]

[0083] Among them I a Refers to the calcium, VD, and VK content (mg / g) in the soluble components after intestinal fluid digestion; I b It refers to the content of calcium, VD and VK in the undigested sample (mg / g).

[0084] The results are as follows:

[0085]

[0086] From the results, it can be seen that the utilization rates of calcium, VD and VK in liquid calcium products after ultramicroemulsification are greatly improved.

[0087] Due to the advanced nature of the technical solution of the present invention, it can be widely used in the fields of nutritional health products, pharmaceutical preparations, micro-nano technology and other application fields.

[0088] In the field of nutritional health products, the oral liquid calcium product of the present invention adopts ultra-microemulsification technology, so that calcium ions can be more evenly dispersed in the liquid, thereby improving the utilization rate of calcium, while enhancing the stability and utilization rate of VD and VK, reducing gastric irritation, and having a novel dosage form, convenient administration, and better comprehensive effects. This will greatly meet the market demand for efficient, stable, and convenient calcium supplements, especially in the elderly, children, and those with dysphagia, and has broad application prospects.

[0089] In the field of pharmaceutical preparations, the ultramicroemulsification technology of the present invention can effectively protect vitamin D and vitamin K, making them less likely to degrade during storage and digestion, and greatly improve the utilization rate of VD and VK after self-emulsification. This will promote the development of the pharmaceutical preparation field, especially in improving the stability and balance of drugs, and has important application value.

[0090] In the field of micro-nano technology, the ultra-micro emulsification technology of the present invention is an important technology, which can disperse drugs or nutrients in liquids to form uniform and stable micro-nano emulsions. This will promote the development of micro-nano technology, especially in improving the bioavailability and stability of drugs, reducing side effects, and improving drug dosage forms, and has important application prospects.

[0091] In general, the technology of the present invention has broad application prospects, large market demand, and huge commercial value and social benefits.

[0092] Based on the above ideal embodiments of the present invention, the relevant staff can make various changes and modifications without departing from the technical concept of the present invention through the above description. The technical scope of the present invention is not limited to the contents of the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A method for preparing ultrafine emulsified liquid calcium for improving the utilization rate of calcium, VD and VK, characterized in that: The following steps are involved: Step 1: Add the activated suspended calcium citrate into the emulsifying pot, add 0.1-2 parts of suspending agent, 0.1-1 parts of acidulant, 5-15 parts of sweetener, 0.1-2 parts of flavor, 60-90 parts of water, start the stirring device, and stir evenly; Step 2: Add the self-emulsifying system into the above emulsifying pot and continue stirring until all ingredients are evenly mixed; Step 3: using a high-speed shear emulsifier to treat the mixture obtained in step 2, and obtaining a primary emulsion after the treatment; Step 4: further treating the primary emulsified liquid with a high-pressure homogenizer for 1 to 5 times to obtain ultrafine emulsified liquid calcium.

2. The method for preparing an ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: The suspending agent in step 1 is selected from one or more of xanthan gum and gum arabic, the acidulant is selected from citric acid, and the sweetener is selected from one or more of white sugar, xylitol, steviol glycoside, and fructose.

3. The method for preparing an ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: The self-emulsifying system comprises vitamin D oil, vitamin K oil, emulsifier and co-emulsifier, and the weight proportions are: 20-60 parts of vitamin D oil and vitamin K oil, 30-50 parts of emulsifier and 0-50 parts of co-emulsifier.

4. The method for preparing an ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: The emulsifier is one or more of Tween 20, Tween 80, polyglycerol ester, phospholipid, and sucrose ester, and the auxiliary emulsifier is one or more of propylene glycol and glycerol.

5. The method for preparing an ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: In step 1 and step 2, the speed of the stirring device is set to 60 rpm / min.

6. The method for preparing ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: In step 3, the speed of the high-speed shear emulsifier is set to 5000 rpm / min, and the emulsification time is 30 to 40 minutes.

7. The method for preparing ultramicroemulsified liquid calcium for improving the utilization rate of calcium, VD and VK according to claim 1, characterized in that: In step 4, the pressure of the high-pressure homogenizer is set to 400-800 bar and the number of homogenization times is 3 times.

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