Salt reducing agent produced by using pepper shell waste and method for producing salt reducing agent by using pepper shell waste

Abstract

The invention belongs to the technical field of seasoning preparation, and relates to a salt reducing agent produced from pepper shell waste and a method thereof, the method comprises the following steps: S1) preparing pepper oleoresin: extracting pepper oleoresin ZO from pepper shell waste; s2) preparing a salt reducing agent: dissolving zanthoxylum oil resin ZO in an organic solvent to obtain a ZO solution; dropwise adding the ZO solution into the whey protein isolate solution, and stirring to obtain a mixed solution; and dropwise adding the stirred mixed solution into the sodium caseinate solution, stirring, dispersing, homogenizing and drying to obtain the salt reducing agent. According to the method for producing the salt reducing agent by utilizing the pepper shell waste, the salt reducing agent is obtained by combining the pepper oleoresin and the microcapsule wall material, so that the intake of salt can be reduced, the fragrance of pepper is removed, and no side effect is generated.

Description

Technical Field

[0001] The present invention belongs to the technical field of condiment preparation, and relates to a method for producing a salt-reducing agent from waste prickly ash husks and the salt-reducing agent obtained thereby. Background Art

[0002] In daily life, table salt not only plays a role in anti-corrosion and freshness preservation, but is also an indispensable condiment. Excessive intake of table salt will increase the risk of various diseases such as hypertension, diabetes, cardiovascular diseases and osteoporosis. In recent years, with the implementation of the national "Three Reductions and Three Health" strategy, the awareness of salt reduction among the people has increased. However, due to the pursuit of taste and flavor, the dietary salt intake of Chinese residents is still much higher than the daily recommended intake of the WHO. Therefore, it is of great significance to develop a green and natural salt-reducing agent that can reduce the salt intake without affecting the taste and flavor of food.

[0003] At present, the method for reducing salt intake can refer to the Chinese invention patent with the publication number CN118000401A, which discloses a salt-reducing and salt-intensifying spicy hot pot base material and its preparation method. Pig bone salty peptides are prepared from pig bones, which are not only rich in various nutrients such as amino acids, minerals, and collagen, but also achieve salt intensification and umami enhancement. However, long-term consumption of pig cartilage will increase the burden on the gastrointestinal tract and is likely to cause abdominal pain. Therefore, this method for reducing salt intake is not suitable for long-term use.

[0004] Prickly ash (Zanthoxylum bungeanum Maxim.) is a plant of the Rutaceae family and the Zanthoxylum genus. Prickly ash has the effects of warming the middle and relieving pain, detoxifying and regulating qi, promoting blood circulation and dredging collaterals, and enhancing immunity. Since ancient times, it has been used as a plant with both medicinal and edible properties. Due to sensory interaction, the saltiness can be enhanced through the numbing sensation of prickly ash, thereby reducing the amount of salt added. However, currently, the existing prickly ash-based salt-reducing agents generally have the problem of overly strong characteristic aroma of prickly ash, and the aroma of prickly ash cannot meet the taste requirements of various people. Moreover, in order to minimize the amount of salt added, a large amount of prickly ash needs to be added, which will cause side effects such as getting angry and allergies. At the same time, long-term and excessive consumption of prickly ash will also stimulate the spleen and stomach, causing discomfort symptoms such as abdominal pain and diarrhea, and even damaging liver function, seriously threatening people's physical health. Summary of the Invention

[0005] Aiming at the technical problems of overly strong characteristic aroma and side effects existing in the existing salt-reducing agents, the present invention provides a method for producing a salt-reducing agent from waste prickly ash husks. The salt-reducing agent is obtained by combining oleoresin of prickly ash with a microcapsule wall material, which can reduce salt intake, remove the aroma of prickly ash, and has no side effects.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is:

[0007] A method for producing a salt-reducing agent using waste prickly ash shells, comprising the following steps:

[0008] S1. Prepare prickly ash oleoresin

[0009] Extract prickly ash oleoresin ZO from waste prickly ash shells;

[0010] S2. Prepare the salt-reducing agent

[0011] S2.1. Dissolve the prickly ash oleoresin ZO in an organic solvent to obtain a ZO solution;

[0012] S2.2. Dropwise add the ZO solution into the whey protein isolate solution and stir to obtain a mixed solution;

[0013] S2.3. Dropwise add the well-stirred mixed solution into the sodium caseinate solution, stir, disperse and homogenize, and dry to obtain the salt-reducing agent; the dosage ratio of the prickly ash oleoresin ZO, organic solvent, whey protein isolate solution, and sodium caseinate solution is (0.8 - 1.2) g : (70 - 90) ml : (50 - 70) ml : (50 - 70) ml; the mass concentration of the whey protein isolate solution and the mass concentration of the sodium caseinate solution are both 3.6%.

[0014] Further defined, in step S2.1, the organic solvent is methanol, ethanol or dichloromethane.

[0015] Further defined, in steps S2.2 and S2.3, the stirring time is 2h - 4h.

[0016] Further defined, in step S2.3, the conditions for dispersion and homogenization are: rotation speed 8000r / min - 1000r / min, time 2min - 4min;

[0017] The drying is spray drying, and the conditions for spray drying are: inlet temperature 120°C - 180°C, outlet temperature 60°C - 90°C, air flow pressure 20bar - 40bar, sample injection rate 500mL / h - 1000mL / h.

[0018] Further defined, the preparation of the prickly ash oleoresin ZO in step S1 specifically includes:

[0019] S1.1. Pretreatment of prickly ash shells

[0020] Dry and crush the waste prickly ash shells to obtain prickly ash powder;

[0021] S1.2. Add the prickly ash powder in step S1.1 to absolute ethanol, shake and mix evenly, then extract. Filter and rotary evaporate the obtained extract to extract the prickly ash oleoresin ZO.

[0022] Further limitation: in the step S1.1, the drying includes air drying and drying by baking; the air drying time is 2 to 3 days, and the drying conditions by baking are: temperature 75°C to 85°C, time 8h - 10h.

[0023] Further limitation: in the step S1.2, the mass-volume ratio of pepper powder to absolute ethanol is 1g:(3 - 11)mL; the conditions for shaking are: temperature 22°C to 25°C, time 35min to 40min; the conditions for extraction are: temperature 30°C to 70°C, time 1h to 12h; the conditions for rotary evaporation are: temperature 55°C to 75°C, pressure 230mBar, time 1h to 3h.

[0024] A salt-reducing agent prepared by the method for producing a salt-reducing agent using waste pepper husks as described above.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0026] 1. The present invention combines oleoresin capsici with microcapsule wall materials (whey protein isolate solution and sodium caseinate solution) to obtain a salt-reducing agent, which can reduce salt intake, remove the aroma of pepper, and has no side effects.

[0027] 2. The present invention makes full use of the nutritional value of pepper, deeply explores the salt-reducing and salt-increasing technology of oleoresin capsici, optimizes the embedding technology of oleoresin capsici, removes the characteristic aroma of pepper, and only retains non-volatile substances. The prepared salt-reducing agent has the advantages of reducing salt and increasing saltiness, being rich in nutrition, and being fast and convenient, and can meet the healthy dietary needs of consumers.

[0028] 3. The salt-reducing agent prepared by the present invention can be quickly dissolved in water. After enzymatic hydrolysis, it can increase the adhesion and penetration effect of sodium ions on the tongue surface, quickly reach the taste sensory organs, strongly increase the perception of saltiness, thereby reducing the intake of table salt, which is green and healthy. Description of the Drawings

[0029] Figure 1 It is a schematic diagram of an EEG experiment;

[0030] Figure 2 It is the salt-reducing effect of different pepper salt-reducing agents under different salt addition amounts;

[0031] Figure 3 It is the PSD result of the brain's response to salt-increasing of different concentrations of pepper water between 1 and 50Hz;

[0032] Figure 4 It is the influence of the ratio of material to liquid on the extraction rate of oleoresin capsici;

[0033] Figure 5 It is the influence of the extraction time on the extraction rate of oleoresin capsici;

[0034] Figure 6 Effect of extraction temperature on the extraction rate of Zanthoxylum oil resin

[0035] Figure 7 Effect of rotary evaporation temperature on the extraction rate of Zanthoxylum oil resin Specific embodiments

[0036] The technical solution protected by the present invention will now be described in detail with reference to the embodiments, but this should not be used to limit the protection scope of the present invention.

[0037] The present invention provides a method for producing a salt-reducing agent using waste Zanthoxylum shells, comprising the following steps:

[0038] S1. Prepare Zanthoxylum oil resin

[0039] Extract Zanthoxylum oil resin ZO from waste Zanthoxylum shells.

[0040] The preparation of Zanthoxylum oil resin ZO in step S1 of the present invention specifically includes:

[0041] S1.1. Pretreatment of Zanthoxylum shells

[0042] Dry and crush the waste Zanthoxylum shells to obtain Zanthoxylum powder.

[0043] In step S1.1 of the present invention, drying includes air drying and drying; the air drying time is 2 - 3 days, and the drying conditions are: temperature 75°C - 85°C, time 8h - 10h.

[0044] S1.2. Add the Zanthoxylum powder obtained in step S1.1 to absolute ethanol, shake and mix evenly, then extract. The obtained extract is filtered and concentrated by rotary evaporation to obtain Zanthoxylum oil resin ZO.

[0045] In step S1.2 of the present invention, the ratio of Zanthoxylum powder to absolute ethanol is 1g:(3 - 11)mL.

[0046] In practice, the mass - volume ratio of Zanthoxylum powder to absolute ethanol is 1g:3mL, 1g:5mL, 1g:7mL, 1g:9mL or 1g:11mL. Preferably, the mass - volume ratio of Zanthoxylum powder to absolute ethanol is 1g:9mL.

[0047] In step S1.2 of the present invention, the shaking conditions are: temperature 22°C - 25°C, time 35min - 40min;

[0048] In practice, the shaking temperature is 22°C, 23°C, 24°C or 25°C; the time is 35min, 37min, 38min or 40min; the vacuum evaporation temperature is 55°C, 57°C, 58°C or 60°C, and the time is 1h, 2h or 3h.

[0049] In step S1.2 of the present invention, the extraction conditions are: temperature 30°C to 70°C, time 1h to 12h.

[0050] In implementation, the temperature is 30°C, 40°C, 50°C, 60°C, 70°C, and the time is 1h, 2h, 4h, 6h, 8h, 10h or 12h. Considering that the higher the temperature and the longer the time, the faster the anhydrous ethanol volatilizes and it will affect the properties of the oleoresin. Preferably, the extraction temperature is 40°C to 60°C; the time is 2h to 8h.

[0051] In step S1.2 of the present invention, the conditions for rotary evaporation are: temperature 55°C to 75°C, pressure 230 mBar, time 1h to 3h.

[0052] S2. Preparation of salt-reducing agent

[0053] S2.1. Dissolve the oleoresin ZO of Chinese prickly ash in an organic solvent to obtain a ZO solution;

[0054] S2.2. Dropwise add the ZO solution into the whey protein isolate solution and stir to obtain a mixed solution;

[0055] S2.3. Dropwise add the well-stirred mixed solution into the sodium caseinate solution, and after stirring, dispersion homogenization, and drying, obtain the salt-reducing agent.

[0056] In the present invention, the dosage ratio of the oleoresin ZO of Chinese prickly ash, the organic solvent, the whey protein isolate solution, and the sodium caseinate solution is (0.8 to 1.2) g : (70 to 90) ml : (50 to 70) ml : (50 to 70) ml; the mass concentration of both the whey protein isolate solution and the sodium caseinate solution is 3.6%.

[0057] In step S2.1 of the present invention, the organic solvent is methanol, ethanol or dichloromethane. Preferably, the organic solvent is ethanol because it has lower toxicity and can be miscible with water in any proportion. Preferably, the concentration of ethanol is 40%.

[0058] In steps S2.2 and S2.3 of the present invention, the stirring time is 2h to 4h. Preferably, the stirring time is 2h, 3h or 4h.

[0059] In step S2.3 of the present invention, the conditions for dispersion homogenization are: rotation speed 8000 r / min to 1000 r / min, time 2min to 4min.

[0060] In step S2.3 of the present invention, the drying is spray drying, and the conditions for spray drying are: inlet temperature 120°C to 180°C, outlet temperature 60°C to 90°C, air flow pressure 20 bar to 40 bar, sample injection rate 500 mL / h to 1000 mL / h.

[0061] The following describes the technical solutions protected by the present invention in detail with several sets of embodiments.

[0062] It should be noted that unless otherwise specified, the chemical drugs and reagents used in the following embodiments are all conventional commercially available products in the art.

[0063] Examples 1 to 9

[0064] In Examples 1 to 9 of the present invention, a salt-reducing agent is prepared using oleoresin ZO from Chinese prickly ash, anhydrous ethanol, whey protein isolate solution, and sodium caseinate solution as raw materials. By designing the ratios of the respective raw materials, the dosage ratios of oleoresin ZO from Chinese prickly ash, anhydrous ethanol, whey protein isolate solution, and sodium caseinate solution are optimized.

[0065] In this embodiment, the method for producing a salt-reducing agent using Chinese prickly ash shell waste includes the following steps:

[0066] S1. Preparation of oleoresin ZO from Chinese prickly ash

[0067] Extract oleoresin ZO from Chinese prickly ash shell waste.

[0068] In this embodiment, oleoresin ZO from Chinese prickly ash is prepared by the following method:

[0069] S1.1. Pretreatment of Chinese prickly ash shells

[0070] Place the Chinese prickly ash shell waste in a cool and ventilated place to air dry for 2 to 3 days; load it into an oven, with a screening thickness of 3 - 4 cm, bake at about 80 °C for 8 h, and then crush to obtain Chinese prickly ash powder with a particle size of 60 mesh.

[0071] S1.2. Preparation of oleoresin ZO from Chinese prickly ash

[0072] Add the Chinese prickly ash powder from step S1.1 to anhydrous ethanol, shake and mix well, and then extract. Filter and rotary evaporate and concentrate the obtained extract to obtain oleoresin ZO from Chinese prickly ash.

[0073] Weigh 300 g of Chinese prickly ash, crush it in a pulverizer, add 2700 mL of anhydrous ethanol, shake at 25 °C for 40 min, mix well, extract at 50 °C for 4 h, and obtain an extract after suction filtration; rotary evaporate and concentrate the extract at 55 °C and a pressure of 230 mBar for 2 h to obtain oleoresin ZO from Chinese prickly ash.

[0074] S2. Preparation of the salt-reducing agent

[0075] S2.1. Dissolve oleoresin ZO from Chinese prickly ash in an organic solvent, and fully stir with a magnetic stirrer until completely dissolved to obtain a ZO solution.

[0076] S2.2. Dropwise add the ZO-ethanol solution into the whey protein isolate solution drop by drop, and stir for 3 h to obtain a mixed solution;

[0077] S2.3. Dropwise add the well-stirred mixed solution into the sodium caseinate solution, stir for 3 h to obtain a Zanthoxylum oil resin ZO-WPI / SCN mixture; then disperse and homogenize it at a rotation speed of 8000 r / min for 4 min to obtain a uniform ZO-WPI / SCN emulsion; finally, dry the ZO-WPI / SCN emulsion by spray drying to obtain a salt-reducing agent ZO-WPI / SCN.

[0078] Preferably, the conditions for spray drying are: the inlet temperature is 180 °C, the outlet temperature is 90 °C, the gas flow pressure is 40 bar, and the sample injection rate is 500 mL / h.

[0079] In this example, the organic solvent is 40% absolute ethanol. The mass concentrations of both the whey protein isolate solution and the sodium caseinate solution are 3.6%.

[0080] In this example, the preparation process of the whey protein isolate solution is: weigh 9 g of whey protein isolate (WPI) in 240 mL of distilled water to obtain a whey protein isolate solution.

[0081] In this example, the preparation process of the sodium caseinate solution is: weigh 9 g of sodium caseinate (SCN) in 240 mL of distilled water, and heat it at 60 °C for 5 min after complete dissolution to obtain a sodium caseinate solution.

[0082] In Examples 1 to 9, the dosage ratios of Zanthoxylum oil resin ZO, absolute ethanol, whey protein isolate solution, and sodium caseinate solution are shown in Table 1, and then the embedding rates under different ratios are measured to evaluate the intuitive index of the microcapsule embedding effect.

[0083] In this example, the embedding rate refers to the ratio of the Zanthoxylum oil resin embedded inside the microcapsules to the original added oil amount (M0). Use petroleum ether as the extraction solvent, combine with the rapid extraction method to measure the surface oil content (M2), and use the Soxhlet extraction method to measure the total oil content (M1). The calculation formula for the embedding rate is as follows:

[0084] Embedding rate (%) = (M1 - M2) / M0 × 100%

[0085] The embedding rates are shown in Table 1.

[0086] Table 1 Embedding rates at different ratios

[0087]

[0088] As can be seen from Table 1, according to the ratios of Examples 1 to 9, the encapsulation rate of oleoresin prickly ash ranges from 64.52% to 75.26%, indicating that the method of the present invention can improve the encapsulation rate of oleoresin prickly ash; preferably, when the ratio of Example 2 is adopted, that is, the dosage ratio of oleoresin prickly ash ZO, organic solvent, whey protein isolate solution, and sodium caseinate solution is 1 g: 80 ml: 60 ml: 60 ml, the encapsulation rate of oleoresin prickly ash is the highest.

[0089] Next, the performance of the salt-reducing agent prepared by the present invention and the extraction conditions of oleoresin prickly ash are optimized.

[0090] I. Study on the performance of the salt-reducing agent

[0091] Taking the salt-reducing agent (also known as prickly ash salt-reducing agent) prepared in Example 2 as the research object, the solubility and salinity performance of the salt-reducing agent prepared by the present invention are tested and evaluated.

[0092] 1. Artificial sensory evaluation of the effect of the prickly ash salt-reducing agent on increasing salinity and reducing salt

[0093] (1) Evaluate the dissolution performance of the salt-reducing agent ZO-WPI / SCN prepared in Example 2 in water.

[0094] Oleoresin prickly ash is an oily liquid insoluble in water and soluble in ethanol; however, when 1 g of the prepared salt-reducing agent ZO-WPI / SCN is taken and dissolved in 100 mL of pure water at 25°C and stirred evenly, it can be quickly dissolved, proving that its solubility is good and the dissolution rate is fast.

[0095] (2) Conduct a sensory evaluation of the performance of the salt-reducing agent ZO-WPI / SCN prepared in Example 2 above.

[0096] The specific process of the sensory evaluation is as follows: Select 15 consumers aged between 20 and 25 as the evaluation personnel, and the evaluation personnel should not have diseases with reduced taste sensitivity.

[0097] For the salinity evaluation, 5% brine is used as the blank group, and brines with salt contents of 5%, 10%, 15%, 20%, 25%, 30%, and 35% are set as the control groups respectively. 5%, 10%, 15%, and 20% of the ZO-WPI / SCN salt-reducing agent are added to the blank group to set up the test groups. The test groups are evaluated as having a salinity higher than the control group (+), equal to the control group (=), and lower than the control group (-) relative to the control group. After each sample is evaluated, it is necessary to rinse the mouth with clean water for 10 seconds to ensure that it is not affected by the previous sample. The final salinity result is based on the results of ≥80% of the evaluation personnel, as shown in Table 2 specifically.

[0098] Table 2 Comparison of salinity with different addition amounts of the ZO-WPI / SCN salt-reducing agent

[0099]

[0100] The results in Table 2 show that when the addition amount of the ZO-WPI / SCN salt-reducing agent is 15% in 5% brine, it can be equal to the salinity of 30% in the group without adding essential oil microcapsules. And when the addition amount is 20%, the effect of increasing salinity is not obvious. Even when the addition amount increases or decreases, too high a numbness degree will lead to a significant weakening of the salty sensory intensity. Therefore, the salt-reducing effect of the ZO-WPI / SCN salt-reducing agent is about 25%.

[0101] 2. Verify the salt-reducing ability of the Chinese prickly ash salt-reducing agent through electroencephalogram

[0102] Verify the enhancing effect of the Chinese prickly ash salt-reducing agent on saltiness through electroencephalogram (EEG) and artificial sensory evaluation. As Figure 1 is the schematic diagram of the EEG experiment.

[0103] In the specific test process, set three addition amounts of the Chinese prickly ash salt-reducing agent (0%, 10%, 20%) and four addition amounts of salt (5%, 10%, 15%, 20%) to form different experimental groups. After the subjects tasted the samples with different addition amounts, the EEG equipment was used to record the brain electrical activities, and the signals in the brain regions related to taste perception were focused on. The perceptual changes of saltiness were evaluated by comparing the characteristic frequency band activities and power spectra in the EEG signals. Analysis of variance (ANOVA) was used to compare the differences between the EEG signals and sensory scores at different addition amounts. The key point of the analysis is whether the influence of the Chinese prickly ash salt-enhancing agent at different concentrations on saltiness perception is significant.

[0104] Figure 2 is the scoring result of the behavioral test carried out simultaneously with the EEG. Through Figure 2 it can be obtained that as the addition amount of salt increases, the brine score also increases, and as the content of the Chinese prickly ash salt-reducing agent increases, the salt-enhancing effect gradually increases. However, when the salt content is relatively high (15%, 20%), the salt-enhancing effects of the addition amounts of 10% and 20% of the Chinese prickly ash salt-reducing agent are quite the same. It shows that the Chinese prickly ash salt-reducing agent has a better salt-enhancing effect in brine with a lower concentration, and the salt-enhancing effect is not obvious in brine with a higher concentration. And the Chinese prickly ash salt-reducing agent with a higher concentration has a better salt-enhancing and salt-reducing effect than that with a lower concentration.

[0105] From Figure 3 The EEG results show that as the addition amounts of the Chinese prickly ash salt-enhancing agent and salt increase, the activity of the EEG signals in specific frequency bands increases, especially in the prefrontal and temporal lobe regions. The sensory evaluation results also show that the samples added with the Chinese prickly ash salt-enhancing agent are significantly higher in saltiness perception than the non-added group, and the salt-enhancing effect is more significant at a higher concentration (20%).

[0106] From the correlation analysis of EEG data and sensory evaluation scores, the electroencephalogram activity was positively correlated with the sensory evaluation scores, indicating that EEG can be used as a tool for objectively evaluating saltiness perception. Generally speaking, the addition of the Chinese prickly ash salt enhancer effectively enhanced saltiness perception, especially when the enhancer was used at a lower salt concentration, which could significantly improve the saltiness intensity. This provides a scientific basis for the development and application of the Chinese prickly ash salt enhancer.

[0107] II. Optimization of the extraction of Zanthoxylum oil resin ZO

[0108] Since Zanthoxylum oil resin is one of the main raw materials for preparing the Chinese prickly ash salt-reducing agent, the extraction effect of Zanthoxylum oil resin ZO is crucial in the whole preparation process. Therefore, an optimization study on the extraction process of Zanthoxylum oil resin ZO was carried out.

[0109] The purpose of this study was to extract Zanthoxylum oil resin by the ethanol extraction method, select four key factors: solid-liquid ratio, extraction temperature, extraction time, and rotary evaporation temperature, and take the extraction rate of Zanthoxylum oil resin and the intensity of the numbing taste in sensory evaluation as evaluation indexes, and optimize the best technological conditions for extracting Zanthoxylum oil resin with ethanol by using single-factor experiments and orthogonal experimental designs respectively.

[0110] 1. The extraction of Zanthoxylum oil resin ZO was carried out according to the following steps:

[0111] (1) Pretreatment of Chinese prickly ash shell waste

[0112] After removing impurities from the Chinese prickly ash shell waste, it was pulverized with a pulverizer and passed through a 60-mesh sieve to obtain Chinese prickly ash powder.

[0113] (2) Extraction of Zanthoxylum oil resin

[0114] Accurately weigh the Chinese prickly ash powder into a flask, add absolute ethanol according to a certain solid-liquid ratio, and then extract at different temperatures for different times. After the extract was vacuum filtered, it was concentrated with a rotary evaporator at different rotary evaporation temperatures for 2 h (the pressure of the rotary evaporator was set at 230 mBar unchanged) to obtain Zanthoxylum oil resin, and then weighed. The solid-liquid ratio refers to the mass-volume ratio of Chinese prickly ash powder (solid) to absolute ethanol (liquid).

[0115] 2. Determine the best extraction conditions by single-factor experiments

[0116] (1) Solid-liquid ratio: Under the conditions of an extraction time of 2 h, an extraction temperature of 50 °C, and a set temperature of 60 °C for the rotary evaporator unchanged, change the solid-liquid ratio (g / mL) (which are 1:3, 1:5, 1:7, 1:9, 1:11) respectively. Explore the influence of the solid-liquid ratio on the extraction rate of Zanthoxylum oil resin, repeat three times, and take the average value.

[0117] (2) Extraction time: Under the conditions of a material-liquid ratio of 1:3 (g / mL), an extraction temperature of 50 °C, and a set temperature of 60 °C for the rotary evaporator remaining unchanged, the extraction time was changed (1 h, 2 h, 4 h, 8 h, 12 h respectively). To explore the effect of extraction time on the extraction rate of pepper oleoresin, repeat three times and take the average value.

[0118] (3) Extraction temperature: Under the conditions of a material-liquid ratio of 1:3 (g / mL), an extraction time of 2 h, and a set temperature of 60 °C for the rotary evaporator remaining unchanged, the extraction temperature was changed (30 °C, 40 °C, 50 °C, 60 °C, 70 °C respectively). To explore the effect of extraction temperature on the extraction rate of pepper oleoresin, repeat three times and take the average value.

[0119] (4) Rotary evaporation temperature: Under the conditions of a material-liquid ratio of 1:3 (g / mL), an extraction time of 2 h, and an extraction temperature of 50 °C remaining unchanged, the rotary evaporation temperature was changed (55 °C, 60 °C, 65 °C, 70 °C, 75 °C respectively). To explore the effect of rotary evaporation temperature on the extraction rate of pepper oleoresin, repeat three times and take the average value.

[0120] The influence results of the above four single factors on the extraction rate are respectively as Figure 4 、 Figure 5 、 Figure 6 and Figure 7 shown.

[0121] It can be Figure 4 seen that when the material-liquid ratio (g / mL) is between 1:3 and 1:9, with the increase of the solvent amount, the extraction rate of pepper oleoresin gradually increases, and the extraction rate is the largest when the material-liquid ratio reaches 1:9. After that, even if the solvent amount is increased, the extraction rate no longer increases. It can be known that at first, the solvent is relatively less, the material is more, the contact is not sufficient, and the extraction efficiency is not high. With the increase of the material-liquid ratio, the contact area between the solid and liquid phases increases, and the extraction rate of pepper oleoresin gradually increases; when the material-liquid ratio reaches 1:9 (g / mL), the pepper powder and absolute ethanol are almost completely in contact, and the extraction rate is close to the maximum at this time. Therefore, after that, increasing the material-liquid ratio does not increase the extraction rate, and even the loss may be increased due to the evaporation of the solute along with the solvent. Therefore, within the test range, 1:9 (g / mL) is the optimal material-liquid ratio for the extraction of pepper oleoresin.

[0122] It can be Figure 5It can be seen that within the experimental range, the longer the extraction time, the greater the extraction rate of prickly ash oil resin. When the extraction time is short (1 h), the extraction rate of prickly ash oil resin is low; as the time extends, the solid-liquid two phases can come into full contact, resulting in an increase in the extraction rate. Therefore, within the experimental range, the longer the time, the higher the extraction rate. However, due to the long time, the system being at a high temperature for a long time may affect the properties of prickly ash oil resin. So the extraction time should not be too long. At this time, it is found that when the extraction time is 4 h, the extraction rate of prickly ash oil resin increases significantly. After that, as the extraction time extends, the extraction rate of prickly ash oil resin rises slowly. Therefore, it is better to choose 4 h for the extraction time, which can not only improve the extraction efficiency but also save time more effectively.

[0123] It can be seen from Figure 6 that within the experimental range, with other conditions unchanged, the higher the extraction temperature, the greater the extraction rate of prickly ash oil resin. When the extraction temperature is 60 °C, the extraction rate increases significantly. Therefore, the extraction temperature is 60 °C.

[0124] It can be seen from Figure 7 that when the rotary evaporation temperature varies within 55 - 75 °C, the extraction rate fluctuates within 14.23% - 14.56%. It can be seen that the higher the rotary evaporation temperature, the not-so-greater impact on the extraction rate of prickly ash oil resin. However, considering that high temperature may affect the properties of prickly ash oil resin, the rotary evaporation temperature is 55 °C.

[0125] Based on the above single-factor results, during the extraction of prickly ash oil resin, when the material-liquid ratio is 1:9, the extraction temperature is 60 °C, the extraction time is 4 h, and the rotary evaporation temperature is 55 °C, the extraction rate of prickly ash oil resin is the highest, and the intensity and duration of the numbing taste in the sensory evaluation are better.

[0126] 3. Determining the optimal extraction conditions through orthogonal experiments

[0127] Since during the extraction process, the changes of various factors are related, an orthogonal experiment is designed by combining the above single-factor test results.

[0128] On the basis of the single-factor experiment, an L9(3 4 ) experiment is carried out, using the extraction rate of prickly ash oil resin and the intensity of the numbing taste in the sensory evaluation as evaluation indicators.

[0129] The factor-level table of the orthogonal experiment is shown in Table 3. Then, referring to the above extraction steps of prickly ash oil resin ZO, extraction is carried out with the factors in Table 3, and the extraction rate is calculated. The results are shown in Table 4; then, referring to the above extraction steps of prickly ash oil resin ZO, extraction is carried out with the factors in Table 3, and a sensory evaluation of the intensity of the numbing taste is carried out. The results are shown in Table 5.

[0130] Table 3 Factor-level table

[0131]

[0132] Table 4 Results of Extraction Rate in Orthogonal Experiment

[0133]

[0134] Note: For the experiment condition numbers 1, 2, and 3 in the table, please refer to the orthogonal factor level table (Table 2-3).

[0135] Table 5 Analysis of Results in Orthogonal Experiment Design (Sensory Evaluation)

[0136]

[0137] Referring to Table 4, the order of influence of each factor on the extraction rate of oleoresin is A > C > B > D, that is, solid-liquid ratio > extraction time > extraction temperature > rotary evaporation temperature. From this perspective, the optimal process conditions for extracting oleoresin with ethanol are a solid-liquid ratio of 1:9, an extraction temperature of 40°C, an extraction time of 8 h, and a rotary evaporation temperature of 60°C.

[0138] Referring to Table 5, the order of influence of each factor on the sensory evaluation of the numbing taste of oleoresin is B > D > C > A, that is, extraction temperature > rotary evaporation temperature > extraction time > solid-liquid ratio. From this perspective, the optimal process conditions for extracting oleoresin with ethanol are a solid-liquid ratio of 1:9, an extraction temperature of 50°C, an extraction time of 2 h, and a rotary evaporation temperature of 55°C, or a solid-liquid ratio of 1:7, an extraction temperature of 50°C, an extraction time of 2 h, and a rotary evaporation temperature of 55°C.

[0139] In summary, considering the single-factor results, orthogonal results, and the results of the influence on the numbing taste of oleoresin, the optimal extraction conditions are finally determined as follows: a solid-liquid ratio of 1:9, an extraction temperature of 50°C, an extraction time of 4 h, and a rotary evaporation temperature of 55°C. Under these conditions, the extraction rate of oleoresin is the highest, and the intensity and duration of the numbing taste in the sensory evaluation are better.

[0140] In addition, the salt-reducing agents prepared by the examples other than Example 2 were used for solubility and salinity tests, and the results were the same as or similar to those of the salt-reducing agent prepared in Example 2. It shows that the present invention uses waste prickly ash shells as raw materials, combines the extracted oleoresin with microcapsule wall materials (whey protein isolate solution and sodium caseinate solution) to obtain a prickly ash salt-reducing agent, achieving the purpose of reducing salt and increasing salinity, and can also remove the aroma of prickly ash, meeting the taste requirements of various people.

[0141] Obviously, the above examples are merely illustrations for clearly explaining the technical solutions of the present invention, rather than limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation manners here. And the obvious changes or modifications derived therefrom are still within the protection scope of the present invention.

Claims

1. A method for producing a salt-reducing agent using waste prickly ash husks, characterized in that, It includes the following steps: S1. Prepare zanthoxylum oil resin Extract zanthoxylum oil resin ZO from zanthoxylum shell waste; S2. Prepare a salt-reducing agent S2.

1. Dissolve zanthoxylum oil resin ZO in an organic solvent to obtain a ZO solution; S2.

2. Dropwise add the ZO solution into the whey protein isolate solution and stir to obtain a mixed solution; S2.

3. Dropwise add the well-stirred mixed solution into the sodium caseinate solution, stir, disperse and homogenize, and dry to obtain a salt-reducing agent; the dosage ratio of the zanthoxylum oil resin ZO, organic solvent, whey protein isolate solution, and sodium caseinate solution is (0.8 - 1.2) g : (70 - 90) ml : (50 - 70) ml : (50 - 70) ml; the mass concentration of the whey protein isolate solution and the mass concentration of the sodium caseinate solution are both 3.6%.

2. The method for producing a salt-reducing agent using waste prickly ash husks according to claim 1, characterized in that, In step S2.1, the organic solvent is methanol, ethanol or dichloromethane.

3. The method for producing a salt-reducing agent by using waste prickly ash husks according to claim 1, wherein In steps S2.2 and S2.3, the stirring time is 2 h to 4 h.

4. The method for producing a salt-reducing agent using waste prickly ash husks according to claim 1, wherein In step S2.3, the conditions for dispersion and homogenization are: rotation speed 8000 r / min to 1000 r / min, time 2 min to 4 min; The drying is spray drying, and the conditions for spray drying are: inlet temperature 120°C to 180°C, outlet temperature 60°C to 90°C, air flow pressure 20 bar to 40 bar, and sample injection rate 500 mL / h to 1000 mL / h.

5. The method for producing a salt-reducing agent using waste prickly ash husks according to claim 1, characterized in that, The preparation of zanthoxylum oil resin ZO in step S1 specifically includes: S1.

1. Pretreatment of zanthoxylum shell Dry and crush the zanthoxylum shell waste to obtain zanthoxylum powder; S1.

2. Add the zanthoxylum powder in step S1.1 to anhydrous ethanol, shake and mix evenly, then extract. Filter and rotary evaporate and concentrate the obtained extract to extract zanthoxylum oil resin ZO.

6. The method for producing a salt-reducing agent using waste Zanthoxylum bungeanum husks according to claim 5, characterized in that, In step S1.1, the drying includes air drying and oven drying; the air drying time is 2 to 3 days, and the oven drying conditions are: temperature 75°C to 85°C, time 8 h - 10 h.

7. The method for producing a salt-reducing agent using waste prickly ash husks according to claim 5, characterized in that, In step S1.2, the mass-volume ratio of zanthoxylum powder to anhydrous ethanol is 1 g : (3 - 11) mL; the shaking conditions are: temperature 22°C to 25°C, time 35 min to 40 min; the extraction conditions are: temperature 30°C to 70°C, time 1 h to 12 h; the rotary evaporation conditions are: temperature 55°C to 75°C, pressure 230 mBar, time 1 h to 3 h.

8. A salt-reducing agent prepared by the method for producing a salt-reducing agent using zanthoxylum shell waste as claimed in claim 1.

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