CN113974117A - Chinese prickly ash salt microcapsule compound seasoning and preparation method thereof - Google Patents
Chinese prickly ash salt microcapsule compound seasoning and preparation method thereof Download PDFInfo
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- CN113974117A CN113974117A CN202111244299.1A CN202111244299A CN113974117A CN 113974117 A CN113974117 A CN 113974117A CN 202111244299 A CN202111244299 A CN 202111244299A CN 113974117 A CN113974117 A CN 113974117A
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- wall material
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- cyclodextrin
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- 150000003839 salts Chemical class 0.000 title claims abstract description 78
- 239000003094 microcapsule Substances 0.000 title claims abstract description 54
- 235000011194 food seasoning agent Nutrition 0.000 title claims abstract description 52
- 150000001875 compounds Chemical class 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 241001079064 Zanthoxylum schinifolium Species 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 74
- 235000002566 Capsicum Nutrition 0.000 claims abstract description 68
- 239000006002 Pepper Substances 0.000 claims abstract description 67
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 14
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- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 5
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/72—Encapsulation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Seasonings (AREA)
Abstract
The invention discloses a pepper salt microcapsule compound seasoning and a preparation method thereof. Preparing edible cyclodextrin-metal organic framework material (CD-MOF) from gamma-cyclodextrin and potassium hydroxide, and taking the edible cyclodextrin-metal organic framework material as a microcapsule wall material; adding the wall material into distilled water, stirring and dissolving, adding edible salt, stirring and dissolving to obtain a wall material mixed solution. Dissolving the freeze-dried powder of the pepper extract by hot edible ethanol, then adding the solution into the wall material mixed solution, and carrying out a series of treatments to obtain the pepper salt microcapsule compound seasoning. The invention relates to a zanthoxylum salt microcapsule compound seasoning, which adopts CD-MOF as a wall material, solves the problems of single variety, low added value, poor solubility of simple mixed seasonings and the like of the existing salt products, can effectively realize the slow release of zanthoxylum amide substances and aroma components, has larger loading rate and stronger stability compared with cyclodextrin inclusion compounds, can be applied to the food processing industry and daily life, and has certain economic value.
Description
Technical Field
The invention belongs to the technical field of microcapsules and preparation thereof, and particularly relates to a preparation method of a pepper salt microcapsule compound seasoning and the pepper salt microcapsule compound seasoning prepared by the preparation method.
Background
Zanthoxylum bungeanum (Zanthoxylum bungeanum.) is a well-known spice plant, belonging to the family Dicotyledoneae, family Rutaceae, genus Zanthoxylum, whose mature dried pericarp has a strong spicy flavor, and is widely used for the preparation of cooking seasonings and high-grade essences. The pepper is used as a plant for both medicine and food, and generally takes a numb-flavor substance as a quality index for evaluating the quality of the pepper. The fructus Zanthoxyli is mainly derived from unsaturated fatty acid amide with sanshool and sanshoamides. In the food processing industry, the catering industry and the family cooking in China, the pepper is mainly supplied in the form of pepper granules, pepper powder, pepper oil and the like. However, the current supply form of the peppers has poor solubility, low utilization rate and incapability of efficiently releasing spicy and fragrant components; secondly, the substances of the spicy and fragrant components of the pepper are unstable and are easy to volatilize or automatically oxidize in the storage process, so that the pepper is short in shelf life and difficult to store.
Salt is an indispensable and irreplaceable necessity in people's life, but for a long time, salt products in China are single in variety and low in grade, and cannot meet the increasing demand of people on improving the material level. The method develops various salts with high quality and high added value, and has good development prospect. The existing commercially available salt and pepper products are only obtained by simply and physically mixing common salt and pepper powder, have poor flavor and poor quality stability, and are not beneficial to the sustainable development of salt industry enterprises in China.
The microcapsule technology is a technology of coating solid and liquid core materials with natural or synthetic polymer materials to form micro-particles with a core-shell structure. The microcapsule technology can increase the solubility of the core material, increase the stability of the core material and effectively control the release rate of the core material. Metal Organic Frameworks (MOFs) are an emerging crystalline porous support due to their excellent porosity, high loading capacity and ease of surface modification. Cyclodextrin (CD) is a cyclic oligosaccharide that is often used to construct supramolecular systems due to its inherent uniform cavity and the presence of a large number of-OH groups. CD-MOF is prepared by cyclodextrin, and is safe and edible and applied to food sample inspection and food packaging. However, the use of edible CD-MOF as a food delivery system to increase the stability and bioburden rate of food flavor bioactive compounds is nearly lacking. Therefore, the development of food-grade CD-MOF has important significance in the application range of the food field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method for preparing a pepper salt microcapsule compound seasoning by using CD-MOF as a wall material. The problems of single variety, low added value, poor solubility of simple mixed seasonings and the like of the existing salt products can be effectively solved, the slow release of the Zanthoxylum bungeanum amide substances and the aroma components can be effectively realized, and compared with cyclodextrin inclusion, the Zanthoxylum bungeanum amide slow release salt has the advantages of higher loading rate and higher stability, can be applied to the food processing industry and daily life, and has certain economic value.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a pepper salt microcapsule compound seasoning comprises the following steps:
(1) drying the pepper, crushing the pepper by using a crusher, sieving the pepper by using a 40-mesh sieve, adding edible ethanol according to the material-liquid ratio of 1: 10-30 (g: mL), leaching the pepper for 4-6 h at 60 ℃ by using a stirrer at 200-600 rpm, filtering and combining supernate, concentrating the mixture to 20-30% of the original volume, and freeze-drying the mixture to obtain pepper extract freeze-dried powder;
(2) accurately weighing a certain amount of cyclodextrin and potassium hydroxide, dissolving in ultrapure water, placing in a glass tube, performing ultrasonic treatment for 5min to uniformly disperse the cyclodextrin and the potassium hydroxide, passing through a 0.45-micron water system membrane, transferring to another glass tube, adding absolute ethyl alcohol, slowly adding methanol, diffusing into the solution, incubating at 50 ℃ for 6h, precipitating crystals with MeOH and PEG, centrifuging at 4000rpm, collecting crystal precipitates, washing twice with absolute methyl alcohol, and performing vacuum freeze drying to obtain a cyclodextrin-metal organic framework material (CD-MOF) wall material;
(3) adding the CD-MOF wall material into distilled water, stirring at 40-60 ℃ and 200-600 rpm until the CD-MOF wall material is completely expanded and dissolved, and continuously stirring for 30-40 min to obtain a wall material solution;
(4) adding edible salt into the wall material solution obtained in the step (3), and stirring until the edible salt is fully dissolved to obtain a wall material mixed solution;
(5) dissolving the zanthoxylum bungeanum maxim extract freeze-dried powder obtained in the step (1) by using edible ethanol at 60 ℃, then adding the dissolved zanthoxylum bungeanum maxim extract freeze-dried powder into the wall material mixed solution obtained in the step (4), continuously stirring for 30-40 min under the stirring condition of 200-600 rpm, then standing for 4-6 h at room temperature, and sequentially centrifuging and freeze-drying to obtain the zanthoxylum salt microcapsule compound seasoning.
Further, the cyclodextrin in the step (2) is any one of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin.
Furthermore, the molar mass ratio of the alpha-cyclodextrin to the potassium hydroxide is 1: 6-10.
Furthermore, the molar mass ratio of the beta-cyclodextrin to the potassium hydroxide is 1: 6-10.
Furthermore, the molar mass ratio of the gamma-cyclodextrin to the potassium hydroxide is 1: 6-10.
Further, in the step (2), PEG is any one of PEG-4000, PEG-8000, PEG-10000 and PEG-20000.
Further, the mass volume percentage of the salt and the wall material solution in the step (4) is 10-30%, and a wall material mixed solution is obtained.
Further, the mass ratio of the pepper extract freeze-dried powder added in the step (5) to the wall material is 1: 3-5.
Further, the stirring temperature in the step (5) is 30-60 ℃.
Further, in the step (5), centrifuging for 15-30 min at the rotating speed of 4000-6000 g.
The invention also discloses the zanthoxylum salt microcapsule compound seasoning prepared by the preparation method of any zanthoxylum salt microcapsule compound seasoning.
Further, the embedding rate of the pepper salt microcapsule compound seasoning extract is 63.3-75.5%; after the accelerated storage for 14 days at 50 ℃, the loss rate of the total content of the amide substances of the numb taste components of the Chinese prickly ash is 5.47-19.76%.
The invention has the beneficial effects that:
the preparation method is simple and easy to operate, and the compound seasoning of the pepper salt microcapsule is prepared by adopting CD-MOF as a wall material. According to the invention, the ethanol is adopted to extract the pepper to prepare the pepper extract freeze-dried powder, so that the spicy and fragrant components in the pepper are efficiently extracted, and the utilization rate of the pepper is increased; by adopting a safe and edible CD-MOF embedding technology, the stability and the biological loading rate of the bioactive compound are improved, the slow release of the Zanthoxylum bungeanum amide substances and the aroma components is effectively realized, and the loading rate is higher and the stability is stronger compared with that of a cyclodextrin embedding substance; meanwhile, the pepper salt microcapsule compound seasoning changes the traditional extensive mode of mixing spice powder and salt, can be applied to the food processing industry and daily life, breaks the defects of single product, low additional value and poor product flavor in the salt industry market in China, meets the market demand and has certain economic value.
Drawings
FIG. 1 is an HPLC diagram of amide substances of the pepper salt microcapsule compound seasoning of the invention;
FIG. 2 is a graph of the total content loss rate of amide substances in the spicy component of the zanthoxylum bungeanum in the accelerated storage experiment of the zanthoxylum salt microcapsule compound seasoning for 14 days;
FIG. 3 is a total TIC chart of the aroma components of the pepper salt microcapsule compound seasoning.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention is described in further detail below with reference to specific examples.
Example 1
A preparation method of a pepper salt microcapsule compound seasoning sequentially comprises the following steps:
(1) selecting full-shape and high-quality pepper, drying by hot air at 65 ℃ and 1m/s wind speed, crushing by a crusher, sieving by a 40-mesh sieve, taking 10g of pepper powder, adding 100mL of edible ethanol, leaching for 4h at 200rpm and 60 ℃ on a magnetic stirrer, filtering by a vacuum filter, merging supernate, concentrating by a rotary evaporator to 20% of the original volume, and freeze-drying to obtain pepper extract freeze-dried powder;
(2) accurately weighing 5mM alpha-cyclodextrin and 30mM potassium hydroxide, adding the alpha-cyclodextrin and the 30mM potassium hydroxide into 100mL of distilled water, placing the mixture into a glass tube, performing ultrasonic treatment for 5min to uniformly disperse the mixture, passing through a 0.45 mu m water system film, transferring the mixture into another glass tube, adding absolute ethyl alcohol, slowly adding methanol, diffusing the mixture into the solution, incubating the solution at 50 ℃ for 6h, precipitating crystals by using MeOH and PEG-4000, centrifugally collecting crystal precipitates at 4000rpm, washing the crystal precipitates twice by using absolute methyl alcohol, and performing vacuum freeze drying to obtain the alpha-cyclodextrin-metal organic framework material (alpha-CD-MOF) wall material.
(3) Adding 3g of alpha-CD-MOF wall material into 100mL of distilled water, stirring at 40 ℃ and 200rpm until the alpha-CD-MOF wall material is completely expanded and dissolved, and continuously stirring for 30min to obtain an alpha-CD-MOF wall material solution;
(4) adding 10g of edible salt into the wall material solution obtained in the step (3), and stirring until the edible salt is fully dissolved to obtain a wall material mixed solution;
(5) and (3) taking 1g of the zanthoxylum bungeanum salt extract freeze-dried powder obtained in the step (1), dissolving the zanthoxylum bungeanum salt extract freeze-dried powder with 2mL of edible ethanol at 60 ℃, then adding the dissolved zanthoxylum bungeanum salt freeze-dried powder into the wall material mixed solution obtained in the step (4), continuously stirring the obtained mixture for 35min under the stirring condition of 40 ℃ and 200rpm, then standing the obtained mixture for 6h at room temperature, centrifuging the obtained mixture for 20min at the rotating speed of 4000g, and freeze-drying the obtained product to obtain the zanthoxylum salt microcapsule composite seasoning.
Example 2
A preparation method of a pepper salt microcapsule compound seasoning sequentially comprises the following steps:
(1) selecting full-shape and high-quality pepper, drying by hot air at 65 ℃ and 1m/s wind speed, crushing by a crusher, sieving by a 40-mesh sieve, taking 10g of pepper powder, adding 200mL of edible ethanol, leaching for 5h at 600rpm and 60 ℃ on a magnetic stirrer, filtering by a vacuum filter, merging supernate, concentrating to 25% of the original volume by a rotary evaporator, and freeze-drying to obtain pepper extract freeze-dried powder;
(2) accurately weighing 5mM beta-cyclodextrin and 50mM potassium hydroxide, adding the beta-cyclodextrin and the 50mM potassium hydroxide into 100mL of distilled water, placing the mixture into a glass tube, performing ultrasonic treatment for 5min to uniformly disperse the mixture, passing through a 0.45 mu m water system film, transferring the mixture into another glass tube, adding absolute ethyl alcohol, slowly adding methanol, diffusing the mixture into the solution, incubating the mixture at 50 ℃ for 6h, precipitating crystals by using MeOH and PEG-10000, centrifugally collecting crystal precipitates at 4000rpm, washing the crystal precipitates twice by using absolute methyl alcohol, and performing vacuum freeze drying to obtain the beta-cyclodextrin-metal organic framework material (beta-CD-MOF) wall material.
(3) Adding 5g of beta-CD-MOF wall material into 100mL of distilled water, stirring at 50 ℃ and 400rpm until the beta-CD-MOF wall material is completely expanded and dissolved, and continuously stirring for 40min to obtain a beta-CD-MOF wall material solution;
(4) adding 20g of edible salt into the wall material solution obtained in the step (3), and stirring until the edible salt is fully dissolved to obtain a wall material mixed solution;
(5) and (2) dissolving 1g of the zanthoxylum bungeanum maxim extract freeze-dried powder obtained in the step (1) by using 2mL of 60 ℃ edible ethanol, then adding the dissolved solution into the wall material mixed solution obtained in the step (4), continuously stirring the mixed solution for 30min at the stirring condition of 50 ℃ and 400rpm, then standing the mixed solution for 4h at room temperature, centrifuging the mixed solution for 30min at the rotating speed of 4000g, and freeze-drying the mixed solution to obtain the zanthoxylum salt microcapsule compound seasoning.
Example 3
A preparation method of a pepper salt microcapsule compound seasoning sequentially comprises the following steps:
(1) selecting full-shape and high-quality pepper, drying by hot air at 65 ℃ and 1m/s wind speed, crushing by a crusher, sieving by a 40-mesh sieve, taking 10g of pepper powder, adding 300mL of edible ethanol, leaching for 6h at 600rpm and 60 ℃ on a magnetic stirrer, filtering by a vacuum filter, merging supernate, concentrating by a rotary evaporator to 30% of the original volume, and freeze-drying to obtain pepper extract freeze-dried powder;
(2) accurately weighing 5mM of gamma-cyclodextrin and 40mM of potassium hydroxide, adding the gamma-cyclodextrin and the 40mM of potassium hydroxide into 100mL of distilled water, placing the mixture into a glass tube, performing ultrasonic treatment for 5min to uniformly disperse the mixture, passing through a 0.45 mu m water system film, transferring the mixture into another glass tube, adding absolute ethyl alcohol, slowly adding methanol, diffusing the mixture into the solution, incubating the mixture at 50 ℃ for 6h, precipitating crystals by using MeOH and PEG-20000, centrifugally collecting crystal precipitates at 4000rpm, washing the crystal precipitates twice by using the absolute methyl alcohol, and performing vacuum freeze drying to obtain the wall material of the gamma-cyclodextrin-metal organic framework material (gamma-CD-MOF).
(3) Adding 4g of gamma-CD-MOF wall material into 100mL of distilled water, stirring at 60 ℃ and 500rpm until the materials are completely expanded and dissolved, and continuously stirring for 35min to obtain a gamma-CD-MOF wall material solution;
(4) adding 20g of edible salt into the wall material solution obtained in the step (3), and stirring until the edible salt is fully dissolved to obtain a wall material mixed solution;
(5) and (2) dissolving 1g of the zanthoxylum bungeanum maxim extract freeze-dried powder obtained in the step (1) by using 2mL of 60 ℃ edible ethanol, then adding the dissolved solution into the wall material mixed solution obtained in the step (4), continuously stirring the mixed solution at the temperature of 60 ℃ and the speed of 600rpm for 40min, then standing the mixed solution at room temperature for 4h, centrifuging the mixed solution at the rotating speed of 6000g for 15min, and freeze-drying the mixed solution to obtain the zanthoxylum salt microcapsule compound seasoning.
Comparative example 1
A pepper salt microcapsule compound seasoning is prepared by adopting conventional wall materials, and the preparation method sequentially comprises the following steps:
(1) selecting full-shape and high-quality pepper, drying by hot air at 65 ℃ and 1m/s wind speed, crushing by a crusher, sieving by a 40-mesh sieve, taking 10g of pepper powder, adding 300mL of edible ethanol, leaching for 6h at 600rpm and 60 ℃ on a magnetic stirrer, filtering by a vacuum filter, merging supernate, concentrating by a rotary evaporator to 30% of the original volume, and freeze-drying to obtain pepper extract freeze-dried powder;
(2) adding wall materials (0.25g of gelatin and 0.75g of gamma-cyclodextrin) into 100mL of distilled water, stirring at 60 ℃ and 500rpm until the wall materials are completely expanded and dissolved, and continuously stirring for 35min to obtain a gelatin/gamma-cyclodextrin wall material solution;
(3) adding 30g of edible salt into the gelatin/gamma-cyclodextrin wall material solution in the step (2), and stirring until the edible salt is fully dissolved to obtain a wall material mixed solution;
(4) and (2) taking 0.25g of the zanthoxylum bungeanum maxim extract freeze-dried powder obtained in the step (1), dissolving the zanthoxylum bungeanum maxim extract freeze-dried powder with 2mL of edible ethanol at 60 ℃, then adding the dissolved solution into the wall material mixed solution obtained in the step (3), continuously stirring the mixed solution at 60 ℃ and 600rpm for 40min, then standing the mixed solution at room temperature for 4h, centrifuging the mixed solution at 6000g of rotation speed for 15min, and freeze-drying the mixed solution to obtain the zanthoxylum salt microcapsule compound seasoning.
Experimental example 1
And (4) determining an embedding rate.
Supernatant in the wall material mixed solution of the pepper extract freeze-dried powder of the examples 1-3 and the comparative example 1 is diluted to proper concentration by ethanol, and then the absorbance value at 270nm is measured by a multifunctional microplate reader (SpectraMax, Molecular Devices, USA) to be non-embedded AIs prepared fromDiluting the lyophilized powder of fructus Zanthoxyli extract with ethanol to the same concentration before embedding, and measuring absorbance at 270nm to obtain total amount A of lyophilized powder of fructus Zanthoxyli extractGeneral assembly. The embedding rate was calculated by the following equation (1), and the results are shown in Table 1. Each measurement was carried out at 25 ℃ and biological replicates were carried out at least three times (n.gtoreq.3), and the mean values were used for the analysis, the error being indicated by SD.
Percent of embedding (%) - (A)General assembly-AIs prepared from)/AGeneral assemblyX 100% formula (1)
TABLE 1 encapsulation efficiency of the pepper salt microcapsule seasoning obtained in examples 1 to 3
| Item | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| The embedding rate% | 70.5±0.59 | 63.3±0.27 | 75.5±0.64 | 47.2±0.19 |
As can be seen from the table 1, the pepper salt microcapsule compound seasoning obtained by the invention has a high embedding rate, the highest embedding rate can reach 75.5%, and the embedding rates of examples 1-3 are all higher than that of comparative example 1, which indicates that the loading rate of a cyclodextrin embedding substance is higher.
Experimental example 2
Zanthoxylamide assay experiments were carried out using example 3.
The content of amide substances in the pepper salt microcapsule compound seasoning is measured by the following method. Specifically, the conditions of sample pretreatment and high performance liquid chromatography analysis in the determination method are as follows:
sample pretreatment: accurately weighing 10mg of the pepper salt microcapsule compound seasoning sample into an EP (EP) tube, adding 5mL of ultrapure water, oscillating for 5min, filtering by a 0.22 mu m filter membrane, and detecting by HPLC (high performance liquid chromatography).
Conditions for HPLC analysis: a chromatographic column: MN Nucleodur 1100-5C18 column (
5 μm); mobile phase A: 0.1% formic acid-water solution; mobile phase B: acetonitrile; flow rate: 0.5 mL/min; column temperature: 25 ℃; ultraviolet detection wavelength: 270 nm; sample introduction amount: 20 μ L. The elution procedure is shown in table 2 and the experimental results are shown in fig. 1.
TABLE 2 HPLC elution procedure
| Time (min) | 0 | 40 | 50 | 60 |
| B％ | 35 | 75 | 100 | 35 |
Finally, according to the comparison of retention time and characteristic absorption peaks with the amide standard product, the No. 1-8 peaks in the figure 1 are sequentially determined to be hydroxyl-epsilon-sanshool, hydroxyl-alpha-sanshool, hydroxyl-beta-sanshool, hydroxyl-gamma-sanshool, isosanshool and tetrahydrosanshool.
The peak areas of the 8 amide-based substances are shown in Table 3.
TABLE 38 amide substance peak-out time and peak area
| Peak number | Retention time (min) | Peak area (mAU) |
| 1 | 14.634 | 840.57 |
| 2 | 15.234 | 23402.50 |
| 3 | 15.979 | 2782.61 |
| 4 | 21.532 | 3042.50 |
| 5 | 22.439 | 213.82 |
| 6 | 23.851 | 349.05 |
| 7 | 24.592 | 119.46 |
| 8 | 33.369 | 234.22 |
As can be seen from Table 3, the pepper salt microcapsule compound seasoning obtained by the invention has 8 typical numb-flavor substances of pepper, and maintains the numb-flavor components of the original pepper.
Experimental example 3
Accelerated storage experiments were carried out using the zanthoxylum salt microcapsule complex seasoning obtained in example 3.
The zanthoxylum bungeanum extract freeze-dried powder and 5.0g of the zanthoxylum bungeanum salt microcapsule compound seasoning in the example 3 and the comparative example 1 are accurately weighed, placed in a culture dish and incubated for 14 days in an incubator at 50 ℃ under illumination conditions. Samples are taken once on days 0, 7 and 14, and are respectively dissolved in ethanol and an aqueous solution, the amide substances are diluted by proper times, the method of the experimental example 2 is used for measuring the amide substances, and the peak area sum of the No. 1 to No. 8 peaks of the samples is represented by S. And (3) calculating the loss rate of the amide substances by using the formula (2). Biological replicates were performed at least three times (n.gtoreq.3) and the mean values were used for the analysis, the error being indicated by SD.
Loss ratio (%) of amide-based substance (S)Day 0–S7/14 days)/SDay 0X 100% formula (2)
The results are shown in FIG. 2. In an accelerated storage experiment, the amide substance loss rate of the pepper salt microcapsule compound seasoning is only 0.98% and 1.04% on 7 th and 14 th days, the amide substance loss rate of the pepper salt microcapsule compound seasoning is only 10.89% and 17.38% on 7 th and 14 th days in the current common pepper embedding method comparative example 1, and the amide substance loss rate of the pepper extract freeze-dried powder is up to 69.78% and 97.33% on 7 th and 14 th days.
The pepper salt microcapsule compound seasoning prepared by the invention can effectively reduce the loss rate of amide substances in the product storage process, prolongs the storage period, and has stronger stability compared with cyclodextrin inclusion.
Experimental example 4
The fragrance component measurement experiment was performed on a sample after a 14-day accelerated storage test using the zanthoxylum salt microcapsule compound seasoning obtained in example 3.
The detection adopts Solid Phase Microextraction (SPME) to extract volatile components in the sample, combines GC-MS to analyze the volatile components in the sample, and performs semi-quantification on each main component by an internal standard method (an internal standard substance is ethyl decanoate, and the concentration of an internal standard solution is 1 g/L). All material contents are in equivalents of ethyl decanoate.
Sample pretreatment: accurately weighing 3g of the pepper salt microcapsule compound seasoning sample, 1 mu L of internal standard and 5mL of ultrapure water in a headspace bottle, putting magnetons in the headspace bottle, and immediately sealing the headspace bottle.
Headspace solid phase microextraction conditions: solid phase micro-extraction head: 50/30 μm DVB/CAR/PDMS extraction head. Extraction conditions are as follows: stirring and preheating the headspace bottle filled with the sample at 50 ℃ for 20min, installing an SPME manual sample introduction handle, inserting an 50/30 mu m DVB/CAR/PDMS extraction head into the air part above the headspace bottle, pushing out a fiber head, adsorbing the headspace for 30min, then drawing back the fiber head, inserting the extraction head into a GC sample introduction port, analyzing for 15min, and collecting mass spectrum data.
GC-MS analysis conditions: sample introduction temperature: 250 ℃; a chromatographic column: SH-Rxi-5Sil MS 30m × 0.25mm × 0.25 μm; column temperature procedure: keeping at 60 deg.C for 4min, heating to 200 deg.C at 4 deg.C/min for 1min, heating to 240 deg.C at 3 deg.C/min for 10 min; the carrier gas control mode is as follows: linear velocity; column flow rate: 1 mL/min; and (3) sample introduction mode: shunting; the split ratio is as follows: 20: 1; sample introduction time: 1 min; ion source temperature: 200 ℃; interface temperature: 240 ℃; the collection mode is as follows: scan was used.
The TIC chart of GC-MS is shown in FIG. 3, and the main volatile components and contents thereof are shown in Table 4.
TABLE 4 Main volatile constituents and contents
As can be seen from table 4, 49 main volatile substances (6 alcohols, 7 aldehydes, 1 acid, 11 esters, 20 hydrocarbons and 4 other substances) were co-separated out, wherein the contents of the two substances, i.e., the alcohol and the ester, were the highest, and were 35.26% and 33.86% of the total content, respectively. Therefore, the pepper salt microcapsule compound seasoning prepared by the invention can effectively reduce the loss of fragrance components of pepper in the storage process.
In conclusion, the preparation method is simple and easy to operate, and the pepper salt microcapsule compound seasoning is prepared by adopting a microcapsule technology. The preparation method is simple and easy to operate, and the compound seasoning of the pepper salt microcapsule is prepared by adopting CD-MOF as a wall material. According to the invention, the ethanol is adopted to extract the pepper to prepare the pepper extract freeze-dried powder, so that the spicy and fragrant components in the pepper are efficiently extracted, and the utilization rate of the pepper is increased; by adopting a safe and edible CD-MOF embedding technology, the stability and the biological loading rate of the bioactive compound are improved, the slow release of the Zanthoxylum bungeanum amide substances and the aroma components is effectively realized, and the loading rate is higher and the stability is stronger compared with that of a cyclodextrin embedding substance; meanwhile, the pepper salt microcapsule compound seasoning changes the traditional extensive mode of mixing spice powder and salt, can be applied to the food processing industry and daily life, breaks the defects of single product, low additional value and poor product flavor in the salt industry market in China, meets the market demand and has certain economic value.
The above-described examples are only some, but not all, embodiments of the present invention. All other embodiments and structural changes that can be made by those skilled in the art without inventive effort based on the embodiments described in the present invention or based on the teaching of the present invention, all technical solutions that are the same or similar to the present invention, are within the scope of the present invention.
Claims (10)
1. A preparation method of a pepper salt microcapsule compound seasoning comprises the following steps:
preparing pepper extract freeze-dried powder;
preparing cyclodextrin-metal organic framework material (CD-MOF) wall materials;
adding a CD-MOF wall material into distilled water, stirring and dissolving to obtain a wall material solution;
adding edible salt into the wall material solution, stirring and dissolving to obtain a wall material mixed solution; and
dissolving the freeze-dried powder of the pepper extract by using edible ethanol, and then adding the dissolved freeze-dried powder into the wall material mixed solution to obtain the pepper salt microcapsule compound seasoning;
wherein the cyclodextrin-metal organic framework material (CD-MOF) wall material is prepared by the following method:
dissolving cyclodextrin and potassium hydroxide in a molar mass ratio of 1: 6-10 in ultrapure water, and performing ultrasonic dispersion;
after passing through a 0.45-micron water system film, adding absolute ethyl alcohol and then adding methanol, and diffusing into the solution;
after incubation for 6h at 50 ℃, precipitating crystals with MeOH and PEG, and centrifuging at 4000rpm to collect the crystal precipitate;
washing twice with anhydrous methanol, and vacuum freeze drying to obtain cyclodextrin-metal organic framework material (CD-MOF) wall material.
2. The production method according to claim 1, wherein:
the pepper extract freeze-dried powder is prepared by the following method:
drying the pepper, crushing the pepper by using a crusher, sieving the pepper by using a 40-mesh sieve, adding edible ethanol according to the material-liquid ratio of 1: 10-30 (g: mL), leaching the pepper for 4-6 h at 60 ℃ by using a stirrer at 200-600 rpm, filtering and combining supernate, concentrating the supernate to 20-30% of the original volume, and freeze-drying to obtain the pepper extract freeze-dried powder.
3. The production method according to claim 1, wherein:
the cyclodextrin is any one of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin;
the PEG is any one of PEG-4000, PEG-8000, PEG-10000 and PEG-20000.
4. The production method according to claim 1, wherein:
the wall material solution is prepared by the following method:
adding the CD-MOF wall material into distilled water, stirring at 40-60 ℃ and 200-600 rpm until the wall material is completely expanded and dissolved, and continuously stirring for 30-40 min to obtain a wall material solution.
5. The production method according to claim 1, wherein:
in the preparation of the wall material mixed liquid:
the mass volume percentage of the salt and the wall material solution is 10-30%.
6. The production method according to claim 1, wherein:
the pepper salt microcapsule compound seasoning is prepared by the following method:
dissolving the zanthoxylum bungeanum maxim extract freeze-dried powder by using edible ethanol at 60 ℃, then adding the dissolved zanthoxylum bungeanum maxim extract freeze-dried powder into the wall material mixed solution, continuously stirring for 30-40 min under the stirring condition of 200-600 rpm, then standing for 4-6 h at room temperature, and sequentially centrifuging, freezing and drying to obtain the zanthoxylum bungeanum salt microcapsule compound seasoning.
7. The production method according to claim 6, wherein:
the mass ratio of the pepper extract freeze-dried powder to the wall material mixed liquid is 1: 3-5.
8. The production method according to claim 6, wherein:
the stirring temperature is 30-60 ℃;
the centrifugation conditions were: centrifuging at 4000-6000 g for 15-30 min.
9. A zanthoxylum salt microcapsule compound seasoning prepared by the preparation method according to any one of claims 1 to 8.
10. The zanthoxylum salt microcapsule compound seasoning according to claim 9, wherein:
the embedding rate of the pepper salt microcapsule compound seasoning extract is 63.3-75.5%;
after the accelerated storage for 14 days at 50 ℃, the loss rate of the total content of the amide substances of the numb taste components of the Chinese prickly ash is 5.47-19.76%.
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