Method for preparing oil-soluble zanthoxylum bungeanum oleoresin and water-soluble zanthoxylum bungeanum oleoresin from supercritical zanthoxylum bungeanum oleoresin and application

Abstract

The invention relates to the technical field of food processing, in particular to a method for preparing oil-soluble zanthoxylum oil resin and water-soluble zanthoxylum oil resin from supercritical zanthoxylum oil resin and application of the oil-soluble zanthoxylum oil resin and the water-soluble zanthoxylum oil resin. The method comprises the following steps: uniformly mixing supercritical zanthoxylum oil resin and a salt solution, standing and separating to obtain an upper-layer oil phase and a lower-layer water phase; filtering the upper-layer oil phase, washing a filtering substrate, and mixing filtrate obtained by filtering and washing liquid obtained by washing the filtering substrate to obtain absolute oil; uniformly mixing the absolute oil and a diluent to obtain oil-soluble zanthoxylum oil resin; and uniformly mixing the lower-layer water phase and an emulsion stabilizer to obtain the water-soluble zanthoxylum oil resin. The method has the advantages of being easy to operate, large in treatment scale, low in cost, sufficient in material utilization and capable of being applied industrially, numb-taste substances in the oil-soluble zanthoxylum oil resin and the water-soluble zanthoxylum oil resin are basically free of loss, even and stable in state, free of crystals and precipitates and convenient to use by food processing enterprises.

Description

Technical Field

[0001] The invention relates to the technical field of food processing, and in particular to a method and application of preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by utilizing supercritical Zanthoxylum bungeanum oleoresin. Background Art

[0002] Sichuan pepper is one of the most commonly used spice seasonings in food processing. At present, food processing companies use Sichuan pepper in the following ways: crushing the pepper and using it directly; soaking and extracting it in vegetable oil to make Sichuan pepper oil and then using it; using steam to distill the Sichuan pepper aromatic oil and then using it; using solvent method or supercritical CO 2 It is used after extraction and preparation of pepper oleoresin. Among them, pepper oleoresin refined products are gradually accepted by food processing companies due to their advantages such as convenient storage, high concentration, and standard content of flavor substances. In particular, supercritical pepper oleoresin is favored by the majority of food processing companies because of its low extraction temperature, pure natural and solvent-free, and flavor close to the original pepper fruit.

[0003] Supercritical Zanthoxylum bungeanum oleoresin usually has the problem of easy precipitation due to high concentration, mainly because the content of zanthoxylum bungeanum in the resin product is high and the pectin in the prickly ash fruit is enriched, which easily leads to pectin precipitation due to pectin aggregation and further causes the precipitation of zanthoxylum bungeanum. To solve this problem, some existing technologies proposed either require the use of a large amount of solvent and cause large product loss, or have limited processing capacity and cannot be applied on a large scale, or the resulting product has a limited stability period.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] The object of the present invention is to provide a method and application of preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin. The method has the advantages of simple operation, large processing scale, low cost, full utilization of materials, and industrial application. The prepared product has high stability and uniform state.

[0006] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0007] One aspect of the present invention relates to a method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin, comprising the following steps:

[0008] (a) mixing supercritical Zanthoxylum bungeanum oleoresin and salt solution, leaving to stand and separating to obtain upper oil phase and lower aqueous phase;

[0009] (b) filtering the upper oil phase, washing the filter matrix, mixing the filtrate obtained by the filtration with the washing solution obtained by washing the filter matrix to obtain the clean oil; mixing the clean oil with a diluent to obtain an oil-soluble Zanthoxylum bungeanum oleoresin;

[0010] (c) mixing the lower aqueous phase and the emulsion stabilizer to obtain water-soluble Zanthoxylum bungeanum oleoresin.

[0011] The method has the advantages of simple operation, large processing scale, low cost, full utilization of materials and industrial application. The numbing substances in the obtained oil-soluble Zanthoxylum oleoresin and water-soluble Zanthoxylum oleoresin are basically not lost and are in a uniform and stable state without crystallization and precipitation, which is convenient for use by food processing enterprises.

[0012] Preferably, the salt solution accounts for 0.5% to 5% of the mass of the supercritical Zanthoxylum bungeanum oleoresin.

[0013] Preferably, the concentration of the salt solution is 0.5wt% to 2wt%.

[0014] Preferably, the standing temperature is 40-80°C.

[0015] Preferably, the standing time is 1 to 24 hours.

[0016] Preferably, the diluent comprises: at least one of soybean oil, rapeseed oil, peanut oil, cottonseed oil, sesame oil, corn oil, sunflower oil, olive oil or medium chain triglycerides.

[0017] Preferably, the emulsifier stabilizer comprises at least one of Span, Tween, mono- and di-glycerol fatty acid esters, sucrose fatty acid esters, caprylic and capric glyceride, propylene glycol, glycerol, ethanol or saline.

[0018] Preferably, the added amount of the emulsion stabilizer is 0.2 to 4 times the mass of the lower aqueous phase.

[0019] Another aspect of the present invention also relates to a method for improving the stability of supercritical pepper oleoresin, including the method for preparing oil-soluble pepper oleoresin and water-soluble pepper oleoresin by using supercritical pepper oleoresin.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] (1) The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided by the present invention has the advantages of simple operation, large processing scale, low cost, full utilization of materials, and industrial application. The numbing substances in the obtained oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin are basically not lost and are in a uniform and stable state without crystallization and precipitation, which is convenient for use by food processing enterprises.

[0022] (2) The present invention provides a method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin using supercritical Zanthoxylum bungeanum oleoresin. The pectin in the supercritical Zanthoxylum bungeanum oleoresin is fully swollen in a salt solution under appropriate temperature conditions to produce a density difference with the oily component. The oil phase and the water phase are naturally separated by standing. The separated oil phase and water phase are treated differently to finally obtain stable oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin.

[0023] (3) The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided by the present invention includes adding salt solution to supercritical Zanthoxylum bungeanum oleoresin, which can break the ionization equilibrium on the surface of the colloid particles in the supercritical Zanthoxylum bungeanum oleoresin, making it easier for water to combine with the colloid and fully swell, so that the water phase layer maintains a uniform flow state, which is beneficial to production operation and the later preparation of water-soluble Zanthoxylum bungeanum oleoresin. DETAILED DESCRIPTION

[0024] The technical scheme of the present invention will be clearly and completely described below in conjunction with specific embodiments, but it will be appreciated by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work, all belong to the scope of protection of the present invention. If specific conditions are not indicated in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0025] One aspect of the present invention relates to a method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin, comprising the following steps:

[0026] (a) mixing supercritical Zanthoxylum bungeanum oleoresin and salt solution, leaving to stand and separating to obtain upper oil phase and lower aqueous phase;

[0027] (b) filtering the upper oil phase, washing the filter matrix, mixing the filtrate obtained by the filtration with the washing solution obtained by washing the filter matrix to obtain the clean oil; mixing the clean oil with a diluent to obtain an oil-soluble Zanthoxylum bungeanum oleoresin;

[0028] (c) mixing the lower aqueous phase and the emulsion stabilizer to obtain water-soluble Zanthoxylum bungeanum oleoresin.

[0029] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin has the advantages of simple operation, large processing scale, low cost, full utilization of materials and industrial application. The numbing substances in the obtained oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin are basically not lost and are in a uniform and stable state without crystallization and precipitation, so that food processing enterprises can use them conveniently.

[0030] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin comprises the following steps: fully swelling pectin in supercritical Zanthoxylum bungeanum oleoresin in a salt solution under suitable temperature conditions to generate a density difference with the oily component, naturally separating the oil phase and the water phase by standing, and performing different treatments on the separated oil phase and water phase to finally obtain oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin in a stable state.

[0031] Adding salt solution to supercritical prickly ash oleoresin can break the ionization equilibrium on the surface of the colloid particles in the supercritical prickly ash oleoresin, making it easier for water to combine with the colloid and swell fully, so that the water phase layer maintains a uniform flow state, which is beneficial to production operations and the subsequent preparation of water-soluble prickly ash oleoresin.

[0032] The preparation method of the present invention can use any supercritical prickly ash oleoresin product in the art as a raw material to produce and prepare stable oil-soluble prickly ash oleoresin and water-soluble prickly ash oleoresin. Further, the supercritical prickly ash oleoresin includes but is not limited to at least one of: pure supercritical prickly ash oleoresin, supercritical prickly ash oleoresin with a concentration greater than 70% diluted with medium-chain triglycerides, or supercritical prickly ash oleoresin after aromatic components have been separated.

[0033] Furthermore, the salt solution is 0.5% to 5% of the mass of the supercritical prickly ash oleoresin, including but not limited to any one of 0.5%, 1%, 2%, 3%, 4% or 5% or any range between two of them. The mixing ratio of the salt solution and the supercritical prickly ash oleoresin needs to be controlled within a certain range, which can ensure that the pectin in the supercritical prickly ash oleoresin fully absorbs water and swells without the presence of clear water, and ensure that the oil and water phases are fully separated, and there is no residual pectin in the oil phase, and the water phase does not contain oil.

[0034] Furthermore, the salt solution is 2% to 3% of the mass of the supercritical prickly ash oleoresin.

[0035] Further, the concentration of the salt solution is 0.5wt% to 2wt%, including but not limited to any point value of 0.5wt%, 1wt%, 1.5wt% or 2wt% or any range value between the two. The concentration of the salt solution needs to be controlled within a certain range. If the concentration of the solution is too low, it will not break the ionosphere balance on the surface of the colloidal particles and promote the swelling of the colloid. If the concentration is too high, it will lead to emulsification and make the water phase layer contain oil.

[0036] Furthermore, the concentration of the salt solution is 0.9wt% to 1.1wt%.

[0037] Further, the standing temperature is 40-80°C, including but not limited to any point value of 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C or 80°C or any range value between two thereof. Standing at a certain temperature can promote the water absorption and swelling of pectin in the supercritical prickly ash oleoresin and separate it from the oil phase. If the standing temperature is too low, the water absorption and swelling separation time will be prolonged. If the standing temperature is too high, the properties of the colloid will change to a certain extent, the water absorption capacity will decrease, the state after separation will not flow, and it may even be impossible to use it to prepare water-soluble prickly ash oleoresin.

[0038] Furthermore, the standing time is 1 to 24 hours, including but not limited to any one of 1 hour, 4 hours, 8 hours, 12 hours, 16 hours, 20 hours or 24 hours or any range between two of them. When the oil phase and the water phase are fully separated, the standing time can be terminated.

[0039] Furthermore, the filtering matrix is: food-grade silicon dioxide particles.

[0040] Furthermore, the particle size of the silicon dioxide particles is 80-100 mesh, including but not limited to any one of 80 mesh, 85 mesh, 90 mesh, 95 mesh or 100 mesh or a range between any two of them.

[0041] Furthermore, the thickness of the filtration matrix is ​​3-5 cm, including but not limited to any point value of 3 cm, 3.5 cm, 4 cm, 4.5 cm or 5 cm, or a range value between any two of them.

[0042] Filtering the upper oil phase using a filter matrix of specific material and size is beneficial to improving the stability of the oil-soluble Zanthoxylum bungeanum oleoresin.

[0043] The present invention does not specifically limit the type of diluent, and conventional edible oil products in the art can be used to implement the technical solution of the present invention. In some specific embodiments, the diluent includes but is not limited to: at least one of soybean oil, rapeseed oil, peanut oil, cottonseed oil, sesame oil, corn oil, sunflower seed oil, olive oil or medium chain triglycerides.

[0044] The obtained pure oil is tested for its numbness, and a diluent is added to adjust the numbness of the pure oil, thereby obtaining oil-soluble Zanthoxylum bungeanum oleoresins with different numbness specifications and stable state. The amount of the diluent added is adaptively adjusted according to the numbness of the target product.

[0045] The degree of numbness of the pure oil is tested by ultraviolet spectrophotometry. The specific testing method can refer to the standard method in the industry.

[0046] Furthermore, the emulsion stabilizer includes but is not limited to: at least one of Span, Tween, mono- and di-glycerol fatty acid esters, sucrose fatty acid esters, caprylic and capric glyceride, propylene glycol, glycerol, ethanol or saline.

[0047] The numbing degree of the lower aqueous phase is detected by high performance liquid chromatography, and an emulsifier stabilizer is added to adjust the aqueous phase, so as to obtain water-soluble Zanthoxylum bungeanum oleoresins with different numbing degrees and stable state.

[0048] Furthermore, the amount of the emulsion stabilizer added is 0.2 to 4 times the mass of the lower aqueous phase, including but not limited to any point value of 0.2, 0.5, 1, 1.5, 2, 2.5, 3, 3.5 or 4 times or any range value between two of them. The amount of the emulsion stabilizer added is adjusted according to the numbness and stability adaptability of the target product.

[0049] Another aspect of the present invention also relates to a method for improving the stability of supercritical pepper oleoresin, including the method for preparing oil-soluble pepper oleoresin and water-soluble pepper oleoresin by using supercritical pepper oleoresin.

[0050] The numbing degree involved in the present invention is: the total content of pepper numbing elements (pepper amide substances), the unit is mg / g.

[0051] The embodiments of the present invention will be described in detail below in conjunction with the examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. If no specific conditions are specified in the examples, the conditions are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be obtained commercially.

[0052] Example 1

[0053] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided in this embodiment comprises the following steps:

[0054] 1. Take 100 kg of pure supercritical Zanthoxylum bungeanum oleoresin (numbing degree 210 mg / g), put it in a 200-liter stirring steam heating reaction tank, add 3 kg of 1 wt% saline solution, heat it to a material temperature of 50 ° C under stirring, stir well and keep for 30 minutes, turn off stirring, let it stand for 4 hours, and naturally stratify;

[0055] 2. Release the lower aqueous phase layer, which is 8.5 kg in total and is a uniform fluid viscous liquid. The numbing degree detected by high performance liquid chromatography is 230 mg / g. Add 1 kg of Span 80, 4 kg of Tween 80, 0.55 kg of 0.5 wt% saline, 1.5 kg of mono- and di-glycerol fatty acid esters and 4 kg of caprylic and capric glyceride, heat to 50 ° C and mix well to obtain 19.55 kg of stable water-soluble Zanthoxylum oleoresin with a numbing degree of 100 mg / g.

[0056] 3. A 3-cm thick silica particle filter layer was laid in the filter, the upper oil phase layer was passed through the filter, the filter layer was washed with 3 kg of soybean oil, the filtrate and the washing liquid were mixed to obtain 97.3 kg of clean oil, the numbness of the clean oil detected by ultraviolet spectrophotometry was 195.8 mg / g, 93.2 kg of medium-chain triglycerides were added, and 190.5 kg of clear and transparent stable oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0057] Example 2

[0058] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided in this embodiment comprises the following steps:

[0059] 1. Take 100 kg of pure supercritical Zanthoxylum bungeanum oleoresin (numbing degree 210 mg / g), put it in a 200-liter stirring steam heating reaction tank, add 0.5 kg of 2 wt% saline solution, heat to 80 ° C under stirring, stir well and keep for 30 minutes, turn off stirring, let stand for 8 hours, and naturally stratify;

[0060] 2. Release the lower aqueous phase layer, which is 6 kg in total and is a uniform fluid viscous liquid. The numbing degree detected by high performance liquid chromatography is 230 mg / g. Add 1.5 kg sucrose fatty acid ester, 0.5 kg caprylic acid glyceride, 2.3 kg propylene glycol, 1 kg 1wt% concentration saline, 0.5 kg glycerol and 2 kg ethanol, heat to 50 ° C and mix well to obtain 13.8 kg of stable water-soluble prickly ash oleoresin with a numbing degree of 100 mg / g.

[0061] 3. A 3-cm thick silica particle filter layer was laid in the filter, the upper oil phase layer was passed through the filter, the filter layer was washed with 3 kg of soybean oil, the filtrate and the washing liquid were mixed to obtain 97.5 kg of clean oil, the numbness of the clean oil detected by ultraviolet spectrophotometry was 201.2 mg / g, 98.7 kg of soybean oil was added, and 196.2 kg of clear and transparent stable oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0062] Example 3

[0063] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided in this embodiment comprises the following steps:

[0064] 1. Take 100 kg of pure supercritical Zanthoxylum bungeanum oleoresin (numbing degree 208 mg / g), put it in a 200-liter stirring steam heating reaction tank, add 5 kg of 0.5 wt% saline solution, heat it to a material temperature of 40 ° C under stirring, stir well and keep for 30 minutes, turn off stirring, let stand for 2 hours, and naturally stratify;

[0065] 2. Release the lower aqueous phase layer, 10.5 kg in total, and place it in a stainless steel barrel for 4 hours. There is a stratification phenomenon, wherein the upper layer is a uniform fluid viscous paste, 8.6 kg in total, and the lower layer is clear water, 1.9 kg in total. The numbing degree detected by high performance liquid chromatography is: the paste layer is 228 mg / g, and the clear water layer has no numbing degree, which is discarded; add 6.5 kg of mono- and diglycerol fatty acid esters, 0.5 kg of sucrose fatty acid esters and 4 kg of caprylic and capric acid glyceride to the paste layer, heat to 50 ° C and mix thoroughly to obtain 19.6 kg of stable water-soluble prickly ash oleoresin, with a numbing degree of 100 mg / g;

[0066] 3. A 3-cm thick silica particle filter layer was laid in the filter, the upper oil phase layer was passed through the filter, the filter layer was washed with 3 kg of soybean oil, the filtrate and the washing liquid were mixed to obtain 97.5 kg of clean oil, the numbness of the clean oil detected by ultraviolet spectrophotometry was 185.6 mg / g, 90.9 kg of cottonseed oil was added, and 188.4 kg of clear and transparent stable oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0067] Example 4

[0068] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided in this embodiment comprises the following steps:

[0069] 1. Take 100 kg of pure supercritical Zanthoxylum bungeanum oleoresin (numbing degree 210 mg / g), put it in a 200-liter stirring steam heating reaction tank, add 1 kg of 1.5 wt% saline solution, heat to 60 ° C under stirring, stir well and keep for 30 minutes, turn off stirring, let stand for 16 hours, and naturally stratify;

[0070] 2. Release the lower aqueous phase layer, which is 6.5 kg in total and is a uniform fluid viscous liquid. The numbing degree detected by high performance liquid chromatography is 235 mg / g. Add 5.5 kg of Tween 80, 1.3 kg of Span 80, 0.5 kg of 1 wt% saline, 1 kg of propylene glycol and 0.5 kg of glycerol, heat to 50 ° C and mix well to obtain 15.3 kg of stable water-soluble Zanthoxylum oleoresin with a numbing degree of 100 mg / g.

[0071] 3. A 3-cm thick silica particle filter layer was laid in the filter, the upper oil phase layer was passed through the filter, the filter layer was washed with 3 kg of soybean oil, the filtrate and the washing liquid were mixed to obtain 97.5 kg of clean oil, the numbness of the clean oil detected by ultraviolet spectrophotometry was 199.7 mg / g, 97.2 kg of corn oil was added, and 194.7 kg of clear and transparent stable oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0072] Example 5

[0073] The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin provided in this embodiment comprises the following steps:

[0074] 1. Take 100 kg of pure supercritical Zanthoxylum bungeanum oleoresin (numbing degree 202 mg / g), put it in a 200-liter stirring steam heating reactor, add 4 kg of 1.8 wt% saline solution, heat it to 70 ° C under stirring, stir well and keep for 30 minutes, turn off stirring, let stand for 24 hours, and naturally stratify. The material is divided into three layers, an upper oil phase layer, a middle water phase layer and a lower clear water layer;

[0075] 2. Release the lower layer of clear water, 1 kg in total, and discard it after high performance liquid chromatography detection. Release the middle aqueous phase, 8 kg in total, which is a uniform fluid viscous liquid. The high performance liquid chromatography detection numbness is 238 mg / g. Add 5.54 kg of Tween 80, 1.5 kg of caprylic and capric glyceride, 3 kg of propylene glycol, and 1 kg of glycerol. Heat to 50 ° C and mix thoroughly to obtain 19.04 kg of stable water-soluble Zanthoxylum oleoresin with a numbness of 100 mg / g.

[0076] 3. A 3-cm thick silica particle filter layer was laid in the filter, the upper oil phase layer was passed through the filter, the filter layer was washed with 3 kg of soybean oil, the filtrate and the washing liquid were mixed to obtain 98 kg of clean oil, the numbness of the clean oil detected by ultraviolet spectrophotometry was 186.7 mg / g, 85 kg of olive oil was added, and 183 kg of clear and transparent stable oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0077] Example 6

[0078] The difference between this embodiment and embodiment 1 is that in step 1, saline solution with a concentration of 0.3 wt % is added.

[0079] After standing and stratifying, the lower aqueous phase layer was slightly turbid and weighed 8.5 kg. The weight of the oil phase layer after filtering and combining the washing liquid was 97.4 kg. In this embodiment, 19.5 kg of water-soluble Zanthoxylum oleoresin was obtained, and the numbness was 100 mg / g. 190 kg of oil-soluble Zanthoxylum oleoresin was obtained, and the numbness was 100 mg / g.

[0080] Example 7

[0081] The difference between this embodiment and embodiment 1 is that in step 1, saline solution with a concentration of 2.5 wt % is added.

[0082] After standing and stratifying, the lower aqueous phase layer was in the form of an emulsion, weighing 13.2 kg, and the weight of the oil phase layer after filtering and combining the washing liquid was 92.8 kg. In this embodiment, 23.55 kg of water-soluble Zanthoxylum bungeanum oleoresin was obtained, and the numbness was 116.3 mg / g. 186.5 kg of oil-soluble Zanthoxylum bungeanum oleoresin was obtained, and the numbness was 97.9 mg / g.

[0083] Example 8

[0084] The difference between this embodiment and embodiment 1 is that 0.5 kg of saline solution is added in step 1.

[0085] After standing and stratifying, the boundary between the upper oil phase layer and the lower water phase layer is unclear. After separation, there are a few oil droplets on the surface of the lower water phase layer, which is viscous and has poor fluidity. In this embodiment, 17.05 kg of water-soluble prickly ash oleoresin is obtained, and the numbness is 114.6 mg / g. 190.3 kg of oil-soluble prickly ash oleoresin is obtained, and the numbness is 99.8 mg / g.

[0086] Example 9

[0087] The difference between this embodiment and embodiment 1 is that 5 kg of saline solution is added in step 1.

[0088] After standing and stratifying, it presents three layers, with the upper oil phase layer, the middle water phase layer and the lower clear water layer, with clear boundaries. Example 19.55 kg of water-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g. 190.5 kg of oil-soluble Zanthoxylum oleoresin was obtained, with a numbness of 100 mg / g.

[0089] Comparative Example 1

[0090] The difference between this comparative example and Example 1 is that the standing temperature is 35°C. After standing and separating, the boundary is unclear, and the lower aqueous phase layer is slightly turbid. After separation, the weight of the aqueous phase layer is 8.9 kg, and the weight of the oil phase layer after filtering and combining the washing liquid is 97.1 kg. This comparative example obtains 19.95 kg of water-soluble prickly ash oleoresin with a numbness of 102.6 mg / g. 190.1 kg of oil-soluble prickly ash oleoresin is obtained with a numbness of 99.7 mg / g.

[0091] In this comparative example, the separation speed slowed down due to insufficient standing temperature, and the standing time needed to be extended.

[0092] Comparative Example 2

[0093] The difference between this comparative example and Example 1 is that the water added in step 1 is clear water. After standing and stratification, it is divided into three layers, an upper oil phase layer, a middle water phase layer and bottom clear water. After separation or the upper oil phase layer (after filtering and combining the washing liquid), 97.7kg, the middle water phase layer is 7.5kg, and the bottom clear water is 0.8kg. This comparative example obtains 18.55kg of water-soluble prickly ash oleoresin with a numbness of 93mg / g. 190.9kg of oil-soluble prickly ash oleoresin is obtained with a numbness of 101mg / g.

[0094] In this comparative example, due to the absence of salt, the ionization balance on the surface of the colloidal particles cannot be broken, the colloid absorbs water slowly, and the same amount of water cannot be fully absorbed.

[0095] Experimental Example 1

[0096] When adding salt water to supercritical Zanthoxylum bungeanum oleoresin, the effects of different salt water concentrations and different addition amounts on the separation effect are shown in Table 1.

[0097] Table 1

[0098]

[0099] According to the above table, it can be seen that the best concentration of saline solution is about 1wt%, and the best amount of saline solution added is about 3%.

[0100] Experimental Example 2

[0101] The stability of the oily Zanthoxylum bungeanum oleoresin and the water-soluble Zanthoxylum bungeanum oleoresin obtained in each embodiment and comparative example was tested, and the obtained data are shown in Table 2.

[0102] Table 2

[0103]

[0104]

[0105] As can be seen from Table 2, in the embodiment where the amount of water added is less than 3%, the colloid does not absorb water and swell sufficiently; in the embodiment where the concentration of salt water added is less than 1wt%, the colloid absorbs water slowly and does not achieve sufficient swelling and separation; a standing temperature lower than 50°C will result in a longer separation time, and the oil phase and the water phase layer cannot be fully separated within a certain period. All of the above will result in the inclusion of some colloid in the oil phase layer after separation, thereby causing the stability of the finished oil-soluble prickly ash oleoresin to decrease. Therefore, the optimal amount of salt water added is 3%, the concentration is 1%, and the suitable temperature for standing separation is 50°C.

[0106] Although the present invention has been illustrated and described with specific embodiments, it should be appreciated that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Those skilled in the art should understand that the technical solutions described in the above embodiments may be modified, or some or all of the technical features thereof may be replaced by equivalents without departing from the spirit and scope of the present invention. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention. Therefore, this means that all such replacements and modifications within the scope of the present invention are included in the appended claims.

Claims

1. A method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin, characterized in that: The following steps are involved: (a) mixing supercritical Zanthoxylum bungeanum oleoresin and salt solution, leaving to stand and separating to obtain upper oil phase and lower aqueous phase; (b) filtering the upper oil phase, washing the filter matrix, mixing the filtrate obtained by the filtration with the washing solution obtained by washing the filter matrix to obtain the clean oil; mixing the clean oil with a diluent to obtain an oil-soluble Zanthoxylum bungeanum oleoresin; (c) mixing the lower aqueous phase and the emulsion stabilizer to obtain water-soluble Zanthoxylum bungeanum oleoresin.

2. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The salt solution accounts for 0.5% to 5% of the mass of the supercritical prickly ash oleoresin.

3. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The concentration of the salt solution is 0.5wt% to 2wt%.

4. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The standing temperature is 40-80°C.

5. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The standing time is 1 to 24 hours.

6. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The diluent comprises: at least one of soybean oil, rapeseed oil, peanut oil, cottonseed oil, sesame oil, corn oil, sunflower seed oil, olive oil or medium chain triglycerides.

7. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The emulsifying stabilizer comprises at least one of Span, Tween, mono- and di-glycerol fatty acid esters, sucrose fatty acid esters, caprylic and capric glyceride, propylene glycol, glycerol, ethanol or saline.

8. The method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by supercritical Zanthoxylum bungeanum oleoresin according to claim 1, characterized in that: The added amount of the emulsion stabilizer is 0.2 to 4 times the mass of the lower aqueous phase.

9. A method for improving the stability of supercritical prickly ash oleoresin, characterized in that: The invention comprises the method for preparing oil-soluble Zanthoxylum bungeanum oleoresin and water-soluble Zanthoxylum bungeanum oleoresin by using supercritical Zanthoxylum bungeanum oleoresin as described in any one of claims 1 to 8.

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