Preparation method of zanthoxylum bungeanum essential oil microcapsule chewable tablets with blood fat reducing effect

Abstract

The invention discloses a preparation method of Chinese prickly ash essential oil microcapsule chewable tablets with a blood fat reducing effect, and belongs to the field of functional foods. According to the microcapsule, Chinese prickly ash essential oil extracted by supercritical CO2 is used as a core material, chitosan-sodium alginate complex coacervation is used as a wall material, calcium chloride is used as a cross-linking agent, the Chinese prickly ash essential oil microcapsule is prepared by adopting an extrusion method more suitable for the oil-soluble core material, the property of the microcapsule is stable, functional components of the Chinese prickly ash essential oil can be effectively reserved, and the embedding rate reaches 96.5%. The zanthoxylum bungeanum essential oil microcapsule chewable tablet with the blood fat reducing effect is prepared from the following raw material components in percentage by mass: 4-12% of zanthoxylum bungeanum essential oil microcapsules, 25-45% of skimmed milk powder, 25-45% of a filling agent and 10-26% of erythritol. And the method has high functional food application value.

Description

Technical Field

[0001] The invention relates to the field of functional foods, and in particular to a method for preparing a prickly ash essential oil microcapsule chewable tablet with blood lipid lowering effect. Background Art

[0002] Zanthoxylum bungeanum essential oil is a volatile substance with a small molecular weight separated from Zanthoxylum bungeanum. Zanthoxylum bungeanum essential oil has high purity, is cheap and easy to obtain, and is mainly composed of olefin compounds, alcohol compounds, ketone compounds and ester compounds. It has certain effects such as lowering blood lipids and anti-oxidation. Zanthoxylum bungeanum essential oil is unstable under conditions such as high temperature, high pressure and high oxygen during processing, and has a large pungent odor. Microencapsulation can greatly reduce the oxidation and volatilization of essential oils and improve stability. However, in the prior art, microcapsules mostly use a single wall material and a chemical encapsulation method. The mechanical strength of the microcapsules is low, and the embedding rate is generally around 85% to 90%. The effect is not ideal, and the preparation method often damages the volatile components of the essential oils.

[0003] Blood lipids mainly include triglycerides, cholesterol and its esters, etc. Hyperlipidemia has become the most serious disease that endangers people's health. For chronic diseases, in the prior art, the products used for treatment are mostly drugs, which are not suitable for special groups such as the elderly and children. The human body has weak adaptability, and most drugs have certain side effects. At present, there is no functional food with blood lipid-lowering effect developed using pepper essential oil as a raw material. Summary of the invention

[0004] In view of the above-mentioned prior art, the purpose of the present invention is to provide a method for preparing a Zanthoxylum bungeanum essential oil microcapsule chewable tablet with blood lipid lowering effect. The method for preparing Zanthoxylum bungeanum essential oil microcapsules provided by the present invention has a high embedding rate of Zanthoxylum bungeanum essential oil, a simple preparation process, and good storage stability. The Zanthoxylum bungeanum essential oil microcapsule chewable tablet prepared on the basis of preparing Zanthoxylum bungeanum essential oil microcapsules has the ability to adsorb sodium taurocholate, sodium glycocholate and cholesterol in vitro, and has a good blood lipid lowering effect.

[0005] To achieve the above object, the present invention adopts the following technical solution:

[0006] In a first aspect, the present invention provides a Zanthoxylum bungeanum essential oil microcapsule, wherein the mass ratio of the core material to the wall material in the Zanthoxylum bungeanum essential oil microcapsule is 1:(1-5);

[0007] The core material is prickly ash essential oil extracted by supercritical CO2, and the wall material is composed of chitosan and sodium alginate complex coagulation in a mass ratio of 1:(1-8).

[0008] The second aspect of the present invention provides a method for preparing the above-mentioned Zanthoxylum essential oil microcapsules, comprising the following steps:

[0009] (1) dissolving chitosan in 1% glacial acetic acid solution, adding anhydrous calcium chloride, adjusting the pH to obtain a chitosan wall material solution, and dissolving sodium alginate in purified water to obtain a sodium alginate wall material solution;

[0010] (2) emulsifying the Zanthoxylum bungeanum essential oil with Tween-80, and then mixing it with the sodium alginate wall material solution to form an essential oil mixed solution by coagulation;

[0011] (3) uniformly dropping the essential oil mixed solution into the stirring chitosan wall material solution to form a microcapsule suspension, filtering to obtain wet microcapsules, and freeze-drying the wet microcapsules to obtain Zanthoxylum essential oil microcapsules.

[0012] The concentration of anhydrous calcium chloride in step (1) is 1% to 5%.

[0013] The pH adjustment treatment in step (1) is to adjust the pH value to 5.4 using 10% NaOH solution.

[0014] The third aspect of the present invention provides the use of the above-mentioned Zanthoxylum essential oil microcapsules in the preparation of blood lipid lowering products.

[0015] The specific performance of lowering blood lipids is: having the ability to adsorb sodium taurocholate, sodium glycocholate and cholesterol in vitro. In a fourth aspect, the present invention provides a Zanthoxylum essential oil microcapsule chewable tablet, comprising the following raw material components in a mass ratio: 4% to 12% Zanthoxylum essential oil microcapsule, 25% to 45% skim milk powder, 25% to 45% filler, and 10% to 26% erythritol.

[0016] Preferably, the Zanthoxylum essential oil microcapsule chewable tablets comprise the following raw material components in the following mass ratios: 6% Zanthoxylum essential oil microcapsules, 40% skim milk powder, 35% filler, and 18% erythritol.

[0017] The prickly ash essential oil microcapsule chewable tablet further comprises the following raw material components in the following mass ratio: 0.5% of citric acid and 0.5% of magnesium stearate.

[0018] The filler is prepared by mixing maltodextrin, microcrystalline cellulose and mannitol in a mass ratio of 4:1:2.

[0019] The method for preparing the Zanthoxylum bungeanum essential oil microcapsule chewable tablets comprises the following steps:

[0020] The raw material components are weighed according to the mass ratio, mixed evenly, and the whole powder is pressed into tablets to prepare the Zanthoxylum bungeanum essential oil microcapsule chewable tablets.

[0021] Beneficial effects of the present invention:

[0022] 1. The present invention adopts a complex coacervation method, an extrusion method, and a freeze-drying method to prepare Zanthoxylum bungeanum essential oil microcapsules. Compared with high-pressure homogenization emulsification and spray drying methods, this method can effectively reduce the loss of functional components of essential oil core materials during the embedding process. The present invention uses sodium alginate and chitosan as wall materials. When preparing Zanthoxylum bungeanum essential oil microcapsules, sodium alginate is first coagulated on the surface of the Zanthoxylum bungeanum essential oil. Sodium alginate can provide a rich network structure to achieve the initial coating of the Zanthoxylum bungeanum essential oil. Calcium chloride is then dissolved in the chitosan solution, and the chitosan wall material prepared after adjusting the pH completes the complex coacervation. Ca 2+ The cross-linking speed with sodium alginate can be controlled to make the microcapsule morphology more complete, the mechanical strength of the sodium alginate compound chitosan wall material is higher, the embedding effect of the pepper essential oil is better, and the embedding rate is as high as 96.5%. In addition, the preparation method of the pepper essential oil microcapsule provided by the present invention also improves the storage stability of the pepper essential oil, effectively retains the unsaturated fatty acid components of the pepper essential oil, and prolongs the shelf life of the microcapsule during storage.

[0023] 2. On the basis of preparing the Zanthoxylum bungeanum essential oil microcapsules, the present invention also prepares the Zanthoxylum bungeanum essential oil microcapsule chewable tablets which have the effect of lowering blood lipids and are easy to carry and take. Compared with the current drugs for treating blood lipid-lowering diseases, the erythritol selected by the functional food does not participate in the metabolism of enzymes, sugars, etc., can be directly discharged from the blood, and is suitable for patients with hyperlipidemia and hypertension. Skim milk powder contains a variety of trace elements, which is suitable for people with hyperlipidemia, and effectively masks the pungent smell of Zanthoxylum bungeanum essential oil. The microcrystalline cellulose in the filler can be used as dietary fiber in low-calorie and low-fat functional foods. The prepared chewable tablets are convenient and portable, have a high sensory acceptance, and have no side effects, providing an application space for the comprehensive utilization of Zanthoxylum bungeanum essential oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a test chart of the effect of wall material ratio on microcapsule embedding efficiency.

[0025] Figure 2 This is a test chart showing the effect of wall-core ratio on microcapsule embedding efficiency.

[0026] Figure 3 This is a test chart showing the effect of cross-linker concentration on microcapsule embedding efficiency.

[0027] Figure 4 This is a test chart for the storage stability of microcapsules.

[0028] Figure 5 This is a test chart showing the effect of raw material addition on the sensory score of chewable tablets.

[0029] Figure 6 This is a test chart showing the effect of the amount of skim milk powder added on the sensory score of chewable tablets.

[0030] Figure 7This is a test chart showing the effect of sweetener addition on the sensory score of chewable tablets.

[0031] Figure 8 This is a test chart showing the effect of filler addition on the sensory score of chewable tablets.

[0032] Fig. 9 This is a graph showing the bile salt adsorption performance of chewable tablets; Fig. 9 A in the middle is the test diagram of the adsorption performance of sodium taurocholate. Fig. 9 B in the figure is the adsorption performance test diagram of sodium glycocholate.

[0033] Fig.10 This is a graph showing the cholesterol adsorption performance test of chewable tablets. DETAILED DESCRIPTION

[0034] It should be noted that the following detailed descriptions are illustrative and are intended to provide further explanation of the present application. Unless otherwise specified, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present application belongs.

[0035] The following detailed description is for illustrative purposes only and is intended to provide further explanation of the present application, rather than to limit the scope of the present invention.

[0036] The sodium alginate used in the examples was purchased from Shanghai Hualan Chemical Technology Co., Ltd.; chitosan was purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0037] The pepper essential oil used in the embodiment is extracted from the laboratory of Shandong Agricultural University. The extraction method is as follows: clean and remove impurities from the dried pepper, dry it in a 60°C oven for 2h, crush the completely dried pepper particles into 60 mesh, and store them for later use. Adjust the CO2 flow rate to 21kg / h, the extraction temperature to 50°C, the extraction time to 2h, and the extraction pressure to 15MPa. After the extraction is completed, collect the pepper essential oil below the separation kettles I and II.

[0038] The mannitol, microcrystalline cellulose, maltodextrin, erythritol, citric acid, magnesium stearate, and skimmed milk powder used in the examples are all food grade.

[0039] Example 1: Preparation of Zanthoxylum bungeanum essential oil microcapsules

[0040] (1) Chitosan powder and sodium alginate powder were weighed and prepared in a mass ratio of 1:3.5, and sodium alginate was dissolved in ultrapure water to prepare a 2wt% sodium alginate wall material solution. The weighed chitosan powder was dissolved in a 1wt% glacial acetic acid solution to form a 0.57wt% chitosan-acetic acid solution, anhydrous calcium chloride was added to make the final concentration of anhydrous calcium chloride in the solution 1.5%, and the pH value of the solution was adjusted to 5.4 with a 10% NaOH solution to obtain a chitosan wall material solution.

[0041] (2) Zanthoxylum bungeanum essential oil was weighed in a mass ratio of 1:3 to sodium alginate powder. Zanthoxylum bungeanum essential oil was mixed with Tween-80 in a mass ratio of 20:1 for emulsification, and then mixed with the sodium alginate solution and stirred continuously for 3 hours to form an essential oil mixed solution.

[0042] (3) Using a syringe (No. 5 needle), the essential oil mixed solution was uniformly dripped into the stirring chitosan wall material solution to form a microcapsule suspension, and the wet microcapsules were filtered to obtain wet microcapsules. The wet microcapsules were placed in a -20°C refrigerator for 24 hours for pre-freezing, and freeze-dried for 24 hours to obtain Zanthoxylum essential oil microcapsules, which were stored in a desiccator.

[0043] Example 2: Preparation of Zanthoxylum bungeanum essential oil microcapsule chewable tablets

[0044] Weigh maltodextrin, microcrystalline cellulose and mannitol according to a mass ratio of 4:1:2, mix them evenly, and obtain a filler. Weigh 6% of the pepper essential oil microcapsules prepared in Example 1, 40% of skim milk powder, 35% of the filler, 18% of erythritol (sweetener), 0.5% of citric acid, and 0.5% of magnesium stearate. According to the above mass ratio of raw material components, fully mix them evenly, use a tableting mold with a diameter of 10 mm to perform full powder tableting, so that the pressure and the thickness of the material are fixed, and prepare pepper essential oil microcapsule chewable tablets.

[0045] Example 3: Single factor investigation and response surface experiment on preparation of Zanthoxylum essential oil microcapsules

[0046] 1. Single factor study on the preparation of Zanthoxylum essential oil microcapsules

[0047] This example specifically examines the effects of wall material ratio, wall-core ratio and crosslinking agent concentration on microcapsule embedding efficiency. In this application, the wall material ratio specifically refers to the mass ratio of sodium alginate powder to chitosan powder, and the wall-core ratio specifically refers to the mass ratio of sodium alginate powder to Zanthoxylum bungeanum essential oil. The embedding efficiency detection method is as follows:

[0048] 0.1 g of the prepared Zanthoxylum bungeanum essential oil microcapsules were placed in 20 ml of a mixture of n-hexane and anhydrous ethanol (mixed in a volume ratio of 4:1), ultrasonically extracted at 60 °C for 30 min, shaken for 2 h, centrifuged at 8000 r / min for 20 min, filtered, and the supernatant was taken. The total oil absorbance of the microcapsules was measured at a wavelength of 275 nm and substituted into the standard equation: y = 0.4885x + 0.0113; R 2 =0.9991, calculate the total oil content N1 of microcapsules.

[0049] Take 0.1g of the prepared Zanthoxylum essential oil microcapsules and dissolve them in 10mL of n-hexane-anhydrous ethanol mixture, shake for 90s, filter and take the supernatant, measure the surface oil absorbance at 275nm, and substitute it into the standard equation: y = 0.4885x + 0.0113; R 2 =0.9991, calculate the microcapsule surface oil content N0.

[0050] Then calculate the embedding rate Y of Zanthoxylum bungeanum essential oil microcapsules according to the following formula.

[0051]

[0052] Where: Y is the embedding rate of Zanthoxylum essential oil microcapsules, %; N1 is the total oil content of microcapsules; N0 is the oil content on the surface of microcapsules.

[0053] (1) The influence of wall material ratio on microcapsule embedding efficiency:

[0054] The sodium alginate concentration was controlled to be 2%, the wall-core ratio was 1:3, and the crosslinking agent concentration was 2%. According to the preparation method provided in Example 1, the effects of the wall-core ratios of 1:1, 1:2, 1:4, 1:6, and 1:8 on the microcapsule embedding efficiency were examined. The results of the effects on the embedding efficiency are shown in Figure 1 As shown in the figure, the embedding rate increases first and then decreases with the increase of wall material ratio. When the wall material ratio is 1:4, the microcapsule embedding rate reaches the maximum, which is 96.6%.

[0055] (2) Effect of wall-core ratio on microcapsule embedding efficiency:

[0056] The wall material ratio was controlled to be 1:4, the cross-linking agent concentration was 2%, and the wall-core ratio was set to 1:1, 1:2, 1:3, 1:4, and 1:5. The effect of embedding rate is shown in Figure 2 The embedding rate first increases and then decreases with the increase of the wall-core ratio. When the wall-core ratio is 1:3, the embedding rate of microcapsules reaches the maximum, which is 96.5%.

[0057] (3) Effect of cross-linking agent concentration on microcapsule embedding efficiency:

[0058] The wall material ratio was controlled to be 1:4, the wall core ratio was 1:3, and the crosslinking agent concentration was set to 1%, 2%, 3%, 4%, and 5%, respectively. The effect of the crosslinking agent concentration on the microcapsule embedding rate was investigated. The results are shown in Figure 3 As shown in the figure, the embedding rate increases first and then decreases with the increase of crosslinking agent concentration. When the crosslinking agent concentration is 2%, the microcapsule embedding rate reaches the maximum, which is 96.0%.

[0059] 2. Response surface experiment

[0060] In order to further optimize the optimal process conditions for Zanthoxylum bungeanum essential oil microcapsules, based on the single factor experiment, the three factors of wall material ratio, wall core ratio and crosslinking agent concentration were used as independent variables to design a three-factor three-level response surface experiment as shown in Table 1. The results of the response surface experiment are shown in Table 2; the results of the variance analysis are shown in Table 3.

[0061] Table 1 Response surface analysis factors and coding levels

[0062]

[0063] Table 2 Response surface experimental design and experimental results

[0064]

[0065]

[0066] Table 3 Analysis of variance of quadratic regression model

[0067]

[0068]

[0069] The optimal process conditions obtained by response surface model analysis were as follows: wall material ratio of 1:3.42, wall core ratio of 1:3.46, crosslinking agent concentration of 1.23%, and the embedding efficiency of Zanthoxylum bungeanum essential oil microcapsules under the optimal conditions was 96.995%. According to the actual experimental conditions and the state of microcapsules, the optimized process was adjusted to a wall material ratio of 1:3.5, a wall core ratio of 1:3, and a crosslinking agent concentration of 1.5%, and three verification experiments were carried out under this experimental condition, and the actual embedding efficiency was 96.50±0.50%.

[0070] Example 4: Storage stability determination of Zanthoxylum bungeanum essential oil and microcapsules

[0071] According to the national standard GB / T 5009.227-2016 "Determination of Peroxide Value in Food", the pepper essential oil and the microcapsules prepared in Example 1 were stored in beakers respectively, titrated with sodium thiosulfate, and the peroxide value was measured every 7 days according to the formula.

[0072]

[0073] Where: Y is the peroxide value of the sample, mmol / kg; V is the volume of the sodium thiosulfate standard solution consumed by the sample, mL; V0 is the volume of the sodium thiosulfate standard solution consumed by the blank sample, mL; m is the mass of the sample, g; c is the concentration of the sodium thiosulfate standard solution, mol / L.

[0074] Among them, the blank sample is the sample without adding essential oil and microcapsules under the same experimental conditions.

[0075] The results of storage stability test are shown in Figure 4 The initial peroxide values ​​of Zanthoxylum bungeanum essential oil and its microcapsule products all meet the national standard limit of 9.85mmol / kg. As can be seen from the figure, after 30 days of storage, the Zanthoxylum bungeanum essential oil is close to the standard limit, while the microcapsules are still far below the standard limit after 30 days of storage. The results show that the preparation of Zanthoxylum bungeanum essential oil microcapsules improves the storage stability of Zanthoxylum bungeanum essential oil.

[0076] Example 5: Comparison of Volatile Components of Zanthoxylum bungeanum Essential Oil and Microcapsules

[0077] At room temperature, GC-MS component analysis was performed on Zanthoxylum bungeanum essential oil and microcapsules stored for 30 days to investigate the effect of microcapsule embedding on the main volatile components of Zanthoxylum bungeanum essential oil. The GC-MS component analysis detection method is as follows:

[0078] (1) Sample pretreatment: First, the solid phase microextraction needle was aged at 270°C for 25 min. 1 mL of Zanthoxylum essential oil and 1 g of the microcapsules prepared in Example 1 were respectively placed in a headspace extraction bottle, and after being in a 60°C water bath for 20 min, the extraction needle was adsorbed in a 60°C water bath for 50 min, and then the extraction needle was quickly inserted into the injection port of the GC-MS coupling instrument and desorbed at 260°C for 6 min.

[0079] (2) Chromatographic conditions: non-polar DB-5MS column (30m×0.25mm×0.25μm), injection port temperature 240℃; program temperature rise: 50℃ for 3min, then increase to 70℃ at a rate of 2℃ / min, then increase to 90℃ at a rate of 1℃ / min, continue for 2min, then increase to 150℃ at a rate of 2℃ / min, and finally increase to 250℃ at a rate of 5℃ / min, continue for 10min. High-purity helium was used as the carrier gas, with a flow rate of 1mL / min; split ratio 40:1.

[0080] (3) Mass spectrometry conditions: interface temperature: 240°C; ion source temperature: 230°C; ionization mode: EI; ionization energy: 70 eV; filament flow rate: 0.2 mA; scanning mass range: 30-500 aum.

[0081] The test results are shown in Table 4. The pepper essential oil stored for 30 days detected 35 main components, and the microcapsules detected 38 main components, and the contents of the main volatile components of the two were somewhat different. The microcapsules retained the functional components of the pepper essential oil to a large extent, such as sabinene, eucalyptol, linalyl acetate, etc. in the microcapsules were not detected in the essential oil, and the contents of oleic acid and sanshool were also increased. In addition, the main functional volatile components in the pepper essential oil were largely retained. The test results show that the pepper essential oil microcapsules prepared by the present invention can extend the antioxidant, antibacterial and hypolipidemic effects of the pepper essential oil to a certain extent, and can effectively retain the biologically active components of the pepper essential oil.

[0082] Table 4 GC-MS analysis of volatile components of Zanthoxylum bungeanum essential oil and microcapsules after storage for 30 days

[0083]

[0084] Example 6: Single factor study and orthogonal experiment for preparation of Zanthoxylum essential oil microcapsule chewable tablets

[0085] 1. Single factor study on the preparation of Zanthoxylum bungeanum essential oil microcapsule chewable tablets

[0086] Determination of the added amount of Zanthoxylum essential oil microcapsules: fixed skim milk powder 40%, filler 35%, sweetener 18%, citric acid 0.5%, magnesium stearate 0.5%; set the added amount of Zanthoxylum essential oil microcapsules to (4% ~ 12%).

[0087] Determination of the amount of skim milk powder added: fixed pepper essential oil microcapsules 6%, filler 35%, sweetener 18%, citric acid 0.5%, magnesium stearate 0.5%; set the amount of skim milk powder added to (25% ~ 45%).

[0088] Determination of the amount of filler added: fixed pepper essential oil microcapsules 6%, skim milk powder 40%, sweetener 18%, citric acid 0.5%, magnesium stearate 0.5%; set the amount of filler added to (25% ~ 45%).

[0089] Determination of sweetener filling amount: fixed pepper essential oil microcapsules 6%, skim milk powder 40%, filler 35%, citric acid 0.5%, magnesium stearate 0.5%; set the sweetener addition amount to (10% ~ 26%).

[0090] (1) Determination of the amount of added Zanthoxylum essential oil microcapsules

[0091] The skim milk powder was fixed at 40%, the filler at 35%, and the sweetener at 18%, and the addition amount of Zanthoxylum essential oil microcapsules was set at 4%, 6%, 8%, 10%, and 12%. Figure 5 , with the highest score of 80.5 when the addition amount was 6%.

[0092] (2) Determination of the amount of skim milk powder added

[0093] The content of Zanthoxylum essential oil microcapsules was fixed at 6%, filler at 35%, and sweetener at 18%, and the amount of skim milk powder added was set at 25%, 30%, 35%, 40%, and 45%. Figure 6 When the amount of skim milk powder added is less than 40%, the milk aroma cannot cover the pungent taste of pepper, and the sensory acceptance is low. When the addition amount is 40%, the milk aroma and pepper taste are neutralized. The formula is further optimized through orthogonal experiments, and it is finally determined that the most suitable amount of milk powder is 40%.

[0094] (3) Determination of the amount of sweetener powder added

[0095] The content of Zanthoxylum essential oil microcapsules was fixed at 6%, filler at 35%, and skim milk powder at 40%. The amount of sweetener added was set at 10%, 14%, 18%, 22%, and 26%. Figure 7 , when the erythritol addition amount was 18%, the sensory score was the highest.

[0096] (4) Determination of the amount of filler powder added

[0097] The content of Zanthoxylum essential oil microcapsules was fixed at 6%, sweetener at 35%, and skim milk powder at 40%, and the amount of filler added was set at 25%, 30%, 35%, 40%, and 45%. Figure 8 Fillers do not directly affect the flavor of chewable tablets, but if there is too little filler, the chewable tablets cannot be formed; if there is too much filler, the chewable tablets will have a rough taste. When the addition amount is 35%, the highest sensory score is 83.5.

[0098] 2. Orthogonal experiment for the preparation of Zanthoxylum bungeanum essential oil microcapsule chewable tablets

[0099] Based on the results of single factor experiments, the present invention designs L9(3 4 ) Orthogonal test (see Table 5) was performed to select the optimal addition range of various raw materials and auxiliary materials. The sensory quality of the chewable tablets was explored through the interaction between various factors. The chewable tablets were scored according to the sensory evaluation criteria in Table 6 to screen out the best formula.

[0100] Table 5 Orthogonal factor level coding table

[0101]

[0102] Table 6 Sensory evaluation standards for chewable tablets

[0103]

[0104] Table 7 shows the effects of raw materials, skim milk powder, sweeteners, and fillers on the sensory scores of chewable tablets. From the R value, it can be seen that the amount of pepper essential oil microcapsules added has the greatest sensory effect on the chewable tablets, followed by skim milk powder, sweeteners, and fillers. The best ratio is represented by the K value. The larger the K value, the better the experimental combination effect. It can be seen from the K value that A-K2 value: 82, B-K3 value 80.5, C-K2 value 79.5, D-K2 value 80.58, that is, the sensory score of the combination of A2B3C2D2 is the highest. Combined with the specific experimental conditions and the range of raw material ratios, the optimal formula ratio is adjusted to 6% of pepper essential oil microcapsules, 40% of skim milk powder, 35% of fillers, and 18% of sweeteners.

[0105] Table 7 Results of orthogonal test of product formula

[0106]

[0107]

[0108] Example 7: Determination of the lipid-lowering ability of chewable tablets

[0109] 1. Experimental Methods

[0110] (1) Determination of bile salt adsorption performance

[0111] Use 0.2mol / L, pH 6.3 phosphate buffer to prepare 10mg / mL pepsin and trypsin solutions, and prepare them for immediate use. Prepare 0.01mol / L hydrochloric acid solution and 0.1mol / L sodium hydroxide solution for later use. Weigh different masses of chewable tablets respectively, add 1mL hydrochloric acid and 3mL pepsin, and incubate at 37°C with constant temperature and shaking for 1h. Then add 4mL trypsin and continue incubation for 1h. Subsequently, add 4mL bile salt solution, shake at 37°C for 1h, centrifuge at 4000r / min for 20min, filter, take 2.5mL of supernatant, add 7.5mL 60% sulfuric acid solution, and water bath at 70°C for 20min. Measure the maximum absorbance at 387nm, and set the treatment without adding chewable tablets under the same experimental conditions as substrate blank, and the treatment without adding bile salts under the same experimental conditions as bile salt blank. Reference formula for calculation of the ability of chewable tablets to adsorb bile salts.

[0112]

[0113] Wherein: Y is the bile salt binding rate, %; A1 is the amount of bile salt added; A2 is the remaining amount of bile salt.

[0114] (1) Determination of cholesterol adsorption performance

[0115] Break up the fresh egg yolk with 9 times ultrapure water and stir until emulsified. Weigh two chewable tablets of different weights into a conical flask, add 5mL of egg yolk solution, stir evenly, adjust the pH value of each solution to 2.0 and 7.0 with 6mol / L HCL and 1mol / L NaOH respectively, simulate the gastrointestinal digestive environment, shake at a constant temperature of 37°C for 2h, centrifuge at 4000r / min for 20min, and filter. Take 100μL of the supernatant respectively, make the volume to 400μL with acetic acid, then add 1.5mL of o-phthalaldehyde solution and 1mL of concentrated sulfuric acid in turn, mix evenly, keep it away from light and let it stand for 10min, and measure the absorbance at 550nm. Replace the egg yolk solution with ultrapure water as a substrate blank. Calculate the cholesterol adsorption capacity according to the formula.

[0116]

[0117] In the formula: Y is the sodium cholesterol binding rate, %; A1 is the amount of cholesterol added; A2 is the remaining amount of cholesterol.

[0118] 2. Experimental results

[0119] (1) Determination of bile salt adsorption capacity

[0120] like Fig. 9 As shown in the figure, when the addition amount is 150mg, the binding rate of sodium taurocholate increases rapidly to 40%. At 240mg, the binding rate reaches 55.4%. The binding rate trend of sodium glycocholate is similar to that of sodium taurocholate. At 150mg, the binding rate increases rapidly. At 240mg, the binding rate reaches 50.5%. The results of the two bile salt binding experiments show that the chewable microcapsules of Zanthoxylum bungeanum essential oil have a good lipid-lowering effect.

[0121] (2) Cholesterol adsorption capacity determination

[0122] like Fig.10 It can be seen that in the simulated intestinal environment (pH = 7), when the chewable tablet addition amount is 240 mg, the cholesterol binding rate reaches 48.3%. In the simulated gastric fluid (pH = 2) environment, the cholesterol binding rate changes slowly, and the maximum binding rate is about 39%. The results show that the cholesterol binding rate of chewable tablets in the intestine is higher than that in gastric fluid.

[0123] This application obtains the best embedding process by optimizing the conditions of microcapsule wall material ratio, wall core ratio, and crosslinking agent concentration. Wall material ratio 1:3.5, wall core ratio 1:3, crosslinking agent concentration 1.5%. Under this process, the storage stability of microcapsules has been significantly improved, and the microcapsule embedding rate has reached 96.5%. The pepper essential oil microcapsule chewing tablets were optimized by orthogonal experiment to obtain the best formula process, with the addition of pepper essential oil microcapsules of 6%, skim milk powder of 40%, sweetener of 18%, and filler of 35%. Under this formula, the chewing tablets are light yellow, uniform in thickness, delicate in taste, long in storage time, and good in sensory acceptance. Through in vitro lipid-lowering assay, it was found that the pepper essential oil microcapsule chewing tablets have the in vitro adsorption capacity of sodium taurocholate, sodium glycocholate, and cholesterol, showing a certain lipid-lowering activity.

[0124] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A Zanthoxylum bungeanum essential oil microcapsule, characterized in that: The mass ratio of the core material to the wall material in the Zanthoxylum bungeanum essential oil microcapsule is 1:(1-5); The core material is prickly ash essential oil extracted by supercritical CO2, and the wall material is composed of chitosan and sodium alginate complex coagulation in a mass ratio of 1:(1-8).

2. The method for preparing the Zanthoxylum bungeanum essential oil microcapsules according to claim 1, characterized in that: The steps include: (1) dissolving chitosan in glacial acetic acid solution, adding anhydrous calcium chloride, adjusting the pH, obtaining a chitosan wall material solution, and dissolving sodium alginate in purified water, obtaining a sodium alginate wall material solution; (2) emulsifying the Zanthoxylum bungeanum essential oil with Tween-80, and then mixing it with the sodium alginate wall material solution to form an essential oil mixed solution by coagulation; (3) uniformly dropping the essential oil mixed solution into the stirring chitosan wall material solution to form a microcapsule suspension, filtering to obtain wet microcapsules, and freeze-drying the wet microcapsules to obtain Zanthoxylum essential oil microcapsules.

3. The preparation method according to claim 2, characterized in that: The concentration of anhydrous calcium chloride in step (1) is 1% to 5%.

4. The preparation method according to claim 2, characterized in that: The pH adjustment treatment in step (1) is to adjust the pH value of the solution to 5.4 using a 10% NaOH solution.

5. Use of the Zanthoxylum essential oil microcapsules according to claim 1 in preparing blood lipid lowering products.

6. The use according to claim 5, characterized in that: The specific performance of lowering blood lipids is: having the ability to adsorb sodium taurocholate, sodium glycocholate and cholesterol in vitro.

7. A chewable tablet of Zanthoxylum bungeanum essential oil microcapsule, characterized in that: The invention comprises the following raw material components in the following mass ratios: 4% to 12% of the pepper essential oil microcapsules according to claim 1, 25% to 45% of skim milk powder, 25% to 45% of a filler, and 10% to 26% of erythritol.

8. The chewable microcapsule tablet of Zanthoxylum bungeanum essential oil according to claim 7, characterized in that: The invention comprises the following raw material components in the following mass ratio: 6% of the pepper essential oil microcapsules according to claim 1, 40% of skim milk powder, 35% of a filler and 18% of erythritol.

9. The Zanthoxylum bungeanum essential oil microcapsule chewable tablet according to claim 7 or 8, characterized in that: The filler is prepared by mixing maltodextrin, microcrystalline cellulose and mannitol in a mass ratio of 4:1:

2.

10. The chewable microcapsule tablet of Zanthoxylum bungeanum essential oil according to any one of claims 7 to 9, characterized in that: The method for preparing the Zanthoxylum bungeanum essential oil microcapsule chewable tablets comprises the following steps: The raw material components are weighed according to the mass ratio, mixed evenly, and the whole powder is pressed into tablets to prepare the Zanthoxylum bungeanum essential oil microcapsule chewable tablets.

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