A method for extracting capsicum oleoresin from fresh industrial capsicum with low energy consumption and low solvent consumption

Abstract

The application discloses a method for extracting capsicum oleoresin from fresh chilli with low energy consumption and low solvent consumption, which takes fresh industrial chilli as raw material, crushes and beats the chilli into pulp, carries out enzymolysis, carries out pressure filtration separation, respectively extracts chilli residue and concentrated chilli water with different solvents, and finally recovers the solvents to obtain capsicum oleoresin. The method can save a large amount of energy consumption of the baking link of industrial chilli, avoid environmental pollution and harm to workers in the powder beating and granulation links, separate chilli residue and water, use the extraction solvent in a targeted manner, extract the concentrated chilli water, and maximize the waste of the solvent, so that the solvent consumption is reduced. The method for extracting capsicum oleoresin has the advantages of simple production process, easy control, low energy consumption, low solvent consumption, safety and environmental protection, and the like, and can improve the comprehensive competitiveness of products and enterprises.

Description

TECHNICAL FIELD

[0001] The present application relates to a method for extracting capsaicin from fresh industrial pepper with low energy consumption and low solvent consumption. BACKGROUND

[0002] Industrial pepper is a pepper variety with 10-20 times the capsaicin content of the common hot pepper, and is mainly used as a raw material for industrial extraction of natural capsaicin. Industrial pepper extract (i.e. capsaicin oleoresin) can be used in food additives, biological medicines, military manufacturing, green pesticides and many other fields, and the demand is huge.

[0003] Industrial pepper has a high capsaicin content and a high extraction added value. At present, the commonly used extraction method on the market is to use dry pepper (pepper) as raw material for extraction. However, there are some problems in the extraction of dry pepper: (1) high cost. Industrial pepper is different from ordinary edible pepper. The surface of the fruit of industrial pepper has a thin film, so it is difficult to dry by natural airing. Only high-temperature baking can be used. The baking cost is about 10-15% of the value of dry pepper from the industry level, which greatly reduces the competitiveness of the product; (2) poor safety. Dry pepper needs to be ground and granulated before extraction, which can easily cause dust pollution. High degree of industrial pepper is more likely to cause harm to the operator's body, and the environmental protection and safety problems are prominent.

[0004] Therefore, some people in the industry have thought of using fresh pepper as raw material to extract capsaicin. For example, the application with publication number CN110156626A discloses a method for extracting capsaicin from fresh pepper. The main technical solution is to cut the fresh pepper into shreds, add an organic solvent for extraction and concentration to obtain a solution containing capsaicin, and then recover the solvent to obtain a capsaicin crude product. The capsaicin crude product is then degummed with ethyl acetate and water, and the gum is separated to obtain a capsaicin extract. However, this process has obvious defects: (1) the process design is unreasonable, and a large amount of solvent is used. Fresh pepper has a high water content. The residue and water are extracted together. Under the premise of a certain material liquid ratio, a large amount of extraction solvent is required, which increases the solvent consumption and cost, and is not conducive to cost reduction and efficiency improvement; (2) the solvent is not used properly. The methanol, ethanol or acetone used is a hydrophilic solvent, which can easily take out the water during the extraction process, increasing the difficulty of subsequent separation and concentration.

[0005] In summary, industrial pepper has a high capsaicin content and a high extraction value. However, the commonly used method for extracting capsaicin oleoresin on the market has some problems, such as unreasonable process design, high energy and solvent consumption, high production cost, unfriendly working environment, poor environmental protection and safety, etc. SUMMARY

[0006] The technical problem to be solved by the present application is to overcome the above-mentioned defects, provide a method for extracting capsicum oleoresin from fresh industrial capsicum with low energy consumption and low solvent consumption, which is simple in process design, can greatly reduce energy consumption, reduce the amount of solvent used, effectively reduce production cost, and improve the environmental protection and safety of the production process.

[0007] The method for extracting capsicum oleoresin from fresh industrial capsicum with low energy consumption and low solvent consumption according to the present application takes fresh industrial capsicum as raw material, and comprises the following steps:

[0008] (1) Slushing the industrial capsicum is broken and slushed to 40-60 meshes to obtain capsicum slurry.

[0009] (2) Enzymolysis 0.05-0.5% of a composite enzyme preparation by weight of the capsicum slurry is added to the capsicum slurry, and the enzyme hydrolysis is carried out at room temperature for not less than 25 minutes to obtain enzyme hydrolyzed capsicum slurry; as a preferred embodiment, the composite enzyme preparation is composed of pectinase, cellulase and protease in a weight ratio of 1:1:1.

[0010] (3) Pressure filtration The enzyme hydrolyzed capsicum slurry is pressure filtered to obtain capsicum residue and capsicum water.

[0011] (4) Capsicum residue extraction The capsicum residue is put into an extraction tank, 10-20 times the weight of the capsicum residue of a composite capsicum residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate and n-hexane is added, and stirring extraction is carried out at 50-60°C for 2-3 hours, and then filtration is carried out to obtain filter residue and extraction liquid A; as a preferred embodiment, the composite capsicum residue extraction solvent is composed of n-butanol, n-hexanol, ethyl acetate and n-hexane in a volume ratio of 4:3:2:1; in order to further recover the solvent, the obtained filter residue is subjected to steam stripping to separate residual solvent and dried residue.

[0012] (5) Capsicum water concentration The capsicum water is transferred into a membrane concentrator, and concentrated to 20-30% of the original volume to obtain capsicum concentrated liquid; as a preferred embodiment, the membrane precision of the membrane concentrator is 200 Da.

[0013] (6) Concentrated liquid extraction The capsicum concentrated liquid is transferred into an extraction tank, 10-20% of the weight of the capsicum concentrated liquid of a composite concentrated liquid extraction solvent composed of n-butanol, n-pentanol and n-hexanol is added, and stirring extraction is carried out at room temperature for 2-3 hours, and then liquid separation is carried out to obtain extraction liquid B and waste water; as a preferred embodiment, the composite concentrated liquid extraction solvent is composed of n-butanol, n-pentanol and n-hexanol in a volume ratio of 1:1:1.

[0014] (7) Desolventization The extraction liquid A and the extraction liquid B are respectively transferred to an evaporator, and the solvent is removed, and then combined to obtain finished capsicum oleoresin.

[0015] Industrial pepper is different from ordinary edible pepper. The surface of the fruit of industrial pepper has a thin film, so it is not easy to dry naturally. In industry, it is dried by high-temperature baking. The baking cost accounts for 10-15% of the value of dried pepper. In addition, the subsequent powdering and granulating processes, the total cost of pretreatment before extraction reaches 20-30% of the value of dried pepper. Industrial pepper is high in pungency, and the powdering and granulating processes pollute the environment and harm the health of the operators, especially the respiratory system. The following is the comparison of baking and pungency of chaitianjiao and industrial pepper:

[0016] 500 grams of fresh chaitianjiao and 500 grams of fresh industrial pepper were taken and placed in an oven. They were baked at 80℃ until the weight was constant. The baking time was recorded and the content of capsaicin in dried pepper was tested. The results are as follows (Table 1):

[0017] Table 1: Comparison of baking and pungency of chaitianjiao and industrial pepper

[0018] Total time to constant weight (h) Capsaicin content in dried chilli (%) Moisture content (%) Cherry pepper 20.5 0.98 75.6 Industrial chilli 72.2 6.67 84.5

[0019] Note: The content of capsaicin was detected according to GB / T21266-2007 Determination of capsaicinoids in peppers and pepper products and method for expressing pungency. Moisture content = (fresh pepper weight - weight when baked to constant weight) ÷ fresh pepper weight.

[0020] From Table 1, it can be seen that the moisture content of industrial pepper is significantly higher than that of chaitianjiao. The time required for baking fresh pepper to constant weight is more than 3.5 times that of chaitianjiao, which is time-consuming and energy-consuming, and greatly affects the efficiency. The content of capsaicin in industrial pepper is much higher than that in chaitianjiao, so industrial pepper is more likely to cause environmental pollution and harm to operators during powdering and granulating.

[0021] The method described in the present application uses fresh industrial pepper as raw material, saves the high cost of baking and drying peppers, reduces the manufacturing cost and time cost, eliminates the need for powdering and granulating, improves environmental friendliness, and ultimately improves the market competitiveness of the product.

[0022] In the method described in the present application, the pepper is beaten and enzymatically hydrolyzed to break the wall, and then filtered under pressure. Different solvents are used to extract different materials from the residue and the liquid. The capsaicin oil resin contained in the pepper residue is slightly fat-soluble, so a composite pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate and n-hexane is used for extraction. The capsaicin oil resin contained in the water is slightly water-soluble, so a composite concentrated liquid extraction solvent composed of n-butanol, n-pentanol and n-hexanol is used for extraction. The pepper residue and water are separated and extracted respectively, and the solvents are used specifically to achieve the best extraction efficiency. The extraction of concentrated pepper water can reduce the amount of solvent used and avoid loss as much as possible, and improve the extraction rate of capsaicin. The composite pepper residue extraction solvent and the composite concentrated liquid extraction solvent are hydrophobic or relatively hydrophobic solvents, and only a small amount of water will be carried out, which is very beneficial to the concentration of the subsequent extraction liquid.

[0023] The method of the present application not only saves a large amount of energy consumption of the industrial pepper baking link, but also avoids environmental pollution and harm to workers in the powdering and granulating links compared with the prior art. The pepper residue and water are separated, the extraction solvent is used in a targeted manner, the pepper water is concentrated and then extracted, solvent waste is maximally avoided, and solvent consumption is reduced. The method of the present application for extracting pepper oleoresin has the advantages of simple production process, low energy consumption, low solvent consumption, safety, environmental protection, etc., and can improve the comprehensive competitiveness of products and enterprises. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 The process flow chart of the method of the present application. DETAILED DESCRIPTION

[0025] The present application will be further described in detail below in combination with examples.

[0026] Example: Pepper oleoresin is extracted from fresh industrial pepper as raw material, and the specific steps are as follows:

[0027] (1) Slurry 500 grams of fresh industrial pepper with a household cell wall breaking machine (brand: Aizela pulverizer 4500) to 40-60 mesh to obtain pepper slurry.

[0028] (2) Enzymolysis Pectinase, cellulase and protease are purchased from the market (Zhejiang Yina Biological Technology Co., Ltd., food grade) and composed into a composite enzyme preparation according to a weight ratio of 1:1:1. 0.5 grams of the composite enzyme preparation is added to the obtained pepper slurry, and the enzyme hydrolysis is carried out at room temperature for 30 minutes to obtain enzyme hydrolyzed pepper slurry.

[0029] (3) Filter pressing The enzyme hydrolyzed pepper slurry is subjected to filter pressing with a fruit and vegetable filter press (hand-operated honey filter press) to obtain 182.5 grams of pepper residue and 315.1 grams of pepper water (loss part is equipment residue).

[0030] (4) Pepper residue extraction The obtained 182.5 grams of pepper residue is put into an extraction tank (5L beaker), 3650 grams of composite pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate and n-hexane according to a volume ratio of 4:3:2:1 (material liquid weight ratio 1:20) is added, and stirring extraction is carried out at 60°C for 3 hours. Filtration (Büchner funnel suction filtration) is carried out to obtain 232.4 grams of filter residue and 3580.1 grams of extraction liquid A (loss part is equipment residue).

[0031] (5) Pepper water concentration step (3) 315.1 g of pepper water obtained is transferred into a rotary evaporator (Zhengzhou Great Wall Scientific Industrial and Trade Co., Ltd. R-1001 / VN), the membrane precision is 200 Da (the molecular weight of capsaicin, the main component of pepper oleoresin, is 305.4, this membrane precision can efficiently concentrate and remove water under the premise of avoiding the loss of capsaicin, and further reduce the manufacturing cost), and concentrated to 90 g, that is, pepper concentrate.

[0032] (6) The 90 g of pepper concentrate obtained by concentrating the concentrate is transferred into a beaker, 18 g of a complex concentrated extraction solvent composed of n-butanol, n-pentanol and n-hexanol in a volume ratio of 1:1:1 is added, and stirred extraction is carried out at room temperature for 3 hours, and then separated by a separating funnel to obtain 16.2 g of extraction liquid B and 90.1 g of waste water.

[0033] (7) The 3580.1 g of extraction liquid A and the 16.2 g of extraction liquid B obtained by desolventizing are respectively transferred into a rotary evaporator (Zhengzhou Great Wall Scientific Industrial and Trade Co., Ltd. R-1001 / VN), and concentrated to remove the solvent at a temperature of 80 ℃ and a pressure of-0.1 MPa; the desolventizing temperature can effectively avoid the pasting of pepper oil caused by high temperature, and the negative pressure state is more conducive to the removal of residual solvent; after the extraction liquid A and the extraction liquid B are desolventized, a total of 19.3 g of pepper oleoresin is obtained, and the capsaicin content is 25.5% (determination method: GB28314-2012 Food Additive Pepper Oleoresin). In this embodiment, 3401 g of solvent is recovered from the pepper residue extraction, and the recovery rate is 95% (3401÷3580=0.95).

[0034] According to the method, the residue and water are extracted separately, and the final product, pepper oleoresin, still contains pepper oleoresin from the pepper residue (extraction liquid A) and the pepper water (extraction liquid B), that is, it contains all different solubilities of pepper oleoresin contained in industrial peppers.

[0035] (8) The 232.4 g of filter residue after the extraction of the pepper residue in step (4) is transferred into a high-temperature oven (an industrial production can use a DTDC steam stripping machine), and dried at 150 ℃ to obtain 58.7 g of dried residue. The filter residue is dried quickly, the residual solvent adsorbed by the filter residue is completely recovered, the solvent loss is minimized, and the dried residue can be used for feed processing, and the utilization of raw materials is maximized.

[0036] In order to prove the effect of the method of the present application relative to the prior art, the following provides a control experiment using a single solvent, different proportions of solvent combinations and different process steps, and the results show that the capsaicin yield and solvent consumption of different methods have obvious differences.

[0037] Comparative Example 1: Pepper residue is extracted with a single solvent-ethanol

[0038] The "pepper residue extraction" step of this comparative example used a single solvent, ethanol (ethanol content greater than 95%), and the remaining steps and processes were identical to the example. Finally, 12.6 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 26.9%.

[0039] Comparative Example 2: Extraction of Pepper Residue Using a Single Solvent, Ethyl Acetate

[0040] The "pepper residue extraction" step of this comparative example used a single solvent, ethyl acetate, and the remaining steps and processes were identical to the example. Finally, 9.5 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 30.5%.

[0041] Comparative Example 3: Extraction of Pepper Water Concentrate Using a Single Solvent, Ethyl Acetate

[0042] The "concentrate extraction" step of this comparative example used a single solvent, ethyl acetate, and the remaining steps and processes were identical to the example. Finally, 9.7 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 37.9%.

[0043] Comparative Example 4: Direct Filter Press Extraction Without Enzymatic Hydrolysis

[0044] This comparative example did not perform enzymatic hydrolysis after pulping the peppers, and the remaining steps and conditions such as extraction solvent were identical to the example. Finally, 8.2 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 31.7%.

[0045] Comparative Example 5: Pepper Residue Extraction with Changed Solvent Ratio (I)

[0046] The "pepper residue extraction" step of this comparative example used a complex pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate, and n-hexane in a volume ratio of 3:3:2:2, and the remaining steps and processes were identical to the example. Finally, 13.1 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 28.6%.

[0047] Comparative Example 6: Pepper Residue Extraction with Changed Solvent Ratio (II)

[0048] The "pepper residue extraction" step of this comparative example used a complex pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate, and n-hexane in a volume ratio of 2:3:2:3, and the remaining steps and processes were identical to the example. Finally, 12.4 g of capsicum oleoresin was obtained by desolventizing, with a capsaicin content of 29.2%.

[0049] Comparative Example 7: Pepper Residue Extraction with Changed Solvent Ratio (III)

[0050] The "pepper residue extraction" step of this comparative example used a composite pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate, and n-hexane in a volume ratio of 1:3:2:4. The remaining steps and processes were the same as in the example. Finally, 12.2 g of pepper oleoresin was obtained by desolventizing, with a capsaicin content of 27.7%.

[0051] Comparative Example 8: Pepper residue extraction, solvent ratio change (four)

[0052] The "pepper residue extraction" step of this comparative example used a composite pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate, and n-hexane in a volume ratio of 1:1:1:1. The remaining steps and processes were the same as in the example. Finally, 13.1 g of pepper oleoresin was obtained by desolventizing, with a capsaicin content of 29.8%.

[0053] Comparative Example 9: Pepper water concentrate extraction, solvent ratio change (one)

[0054] The "concentrate extraction" step of this comparative example used a composite concentrate extraction solvent composed of n-butanol, n-pentanol, and n-hexanol in a volume ratio of 1:2:3. The remaining steps and processes were the same as in the example. Finally, 14.7 g of pepper oleoresin was obtained by desolventizing, with a capsaicin content of 28.4%.

[0055] Comparative Example 10: Pepper water concentrate extraction, solvent ratio change (two)

[0056] The "concentrate extraction" step of this comparative example used a composite concentrate extraction solvent composed of n-butanol, n-pentanol, and n-hexanol in a volume ratio of 3:2:1. The remaining steps and processes were the same as in the example. Finally, 15.6 g of pepper oleoresin was obtained by desolventizing, with a capsaicin content of 24.9%.

[0057] Comparative Example 11: Extraction of pepper residue and water together, testing solvent loss

[0058] In this comparative example, fresh industrial peppers were pulped and enzymatically hydrolyzed without pressure filtration separation, and the pepper residue and water were extracted together. The specific method was as follows:

[0059] (1) Pulping was the same as in the example.

[0060] (2) Enzymatic hydrolysis was the same as in the example.

[0061] (3) The chili pulp after extraction and enzymatic hydrolysis was transferred into a 15 L stainless steel barrel, and 10,000 g of a composite chili residue extraction solvent consisting of n-butanol, n-hexanol, ethyl acetate, and n-hexane in a volume ratio of 4:3:2:1 (solid-liquid ratio 1:20) was added. The mixture was stirred and extracted at 60 ° C for 3 hours, and filtered (Buchner funnel filtration) to obtain 10,315 g of extract (including extraction solvent and chili water). After separation with a separatory funnel, 10,006 g of extract (upper layer) was obtained. The extract was transferred into a rotary evaporator (R-1001 / VN, Zhengzhou Great Wall Science and Technology Industry and Trade Co., Ltd.), concentrated to dryness, and the solvent was recovered to obtain 8,250 g. The recovery rate was 8,250 ÷ 10,000 = 0.825 (82.5%).

[0062] The process differences between the embodiments and the control examples and the results of capsaicin yield are shown in Table 2.

[0063] Table 2: Results of Examples and Comparative Examples

[0064]

[0065]

[0066] Note: "Same" in Table 2 means the process conditions are the same as those in Example.

[0067] Capsaicin yield = (weight of capsicum oleoresin × percentage of capsaicin) ÷ [weight of fresh chili pepper × (1-percentage of water) × percentage of capsaicin in dried chili pepper]

[0068] From the results in Table 2 we can see that:

[0069] (1) The capsaicin yields of Control Examples 1, 2, and 3 are significantly lower than those of the embodiment, indicating that the capsaicin yield is not high when a single solvent is used for extraction, whether in the chili residue extraction or the chili water concentrate extraction process, and the effect on the chili residue extraction is particularly significant; ethanol has a higher polarity and a lower extraction rate for fat-soluble substances, while ethyl acetate has a lower polarity and a lower extraction rate for water-soluble substances. Therefore, a single solvent is significantly less effective than a composite solvent for the extraction of capsaicin with complex components.

[0070] (2) The capsaicin yields of control examples 5, 6, 7, 8, 9, and 10 were significantly lower than those of the embodiments, indicating that regardless of whether the chili residue extraction or the chili water concentrate extraction step is performed, even if a composite extraction solvent is used, the capsaicin yields are different depending on the ratio of each solvent in the composite solvent. The composite solvent ratio in the embodiments of the method of the present invention performs relatively well in both the chili residue extraction and the chili water concentrate extraction steps, and the final capsaicin yield is significantly higher than that of each control example.

[0071] (3) The capsaicin yield of Control Example 4 was significantly lower than that of the Example, indicating that enzymatic hydrolysis plays an important role in the extraction rate of capsicum oleoresin in the method of the present invention.

[0072] (4) Control Example 11 does not perform residue-liquid separation on the pepper pulp, and the solvent usage is as high as 10000 grams at a material-liquid ratio of 1:20, which is 2.7 times more than that of the embodiment, and the solvent recovery rate of Control Example 11 is only 82.5%, which is significantly lower than 95% of the embodiment. The results of Control Example 11 and the embodiment show that the method described in the application has obvious effect on reducing solvent loss, and can reduce a large amount of cost for enterprises and improve product competitiveness in actual production.

[0073] The above are only some embodiments of the application, and the embodiments are only for more clearly illustrating the technical solutions, and are not used for limiting the technical solutions. Those skilled in the art can know from the content of the specification that the technical solutions described in the application can have various implementation manners, as long as the above-mentioned technical solutions are used, all should fall within the protection scope of the application.

Claims

1. A method of extracting oleoresin from fresh industrial chilli with low energy and low solvent consumption, characterized in that, The method takes fresh industrial pepper as raw material, and comprises the following steps: (1) beating pulp The industrial pepper is broken and beaten to 40-60 mesh to obtain pepper pulp; (2) enzymolysis 0.05-0.5% of a compound enzyme preparation by weight of the pepper pulp is added to the pepper pulp, and the mixture is enzymolyzed at room temperature for not less than 25 minutes to obtain enzymolyzed pepper pulp; (3) pressure filtration The enzymolyzed pepper pulp is pressure filtered to obtain pepper residue and pepper water; (4) extraction of pepper residue The pepper residue is put into an extraction tank, 10-20 times by weight of a compound pepper residue extraction solvent composed of n-butanol, n-hexanol, ethyl acetate and n-hexane in a volume ratio of 4:3:2:1 is added, and stirring extraction is carried out at 50-60°C for 2-3 hours, then filtration is performed to obtain filter residue and extraction liquid A; (5) concentration of pepper water The pepper water is transferred into a membrane concentrator, and concentrated to 20-30% of the original volume to obtain pepper concentrated liquid; (6) extraction of concentrated liquid The pepper concentrated liquid is transferred into an extraction tank, 10-20% of a compound concentrated liquid extraction solvent composed of n-butanol, n-pentanol and n-hexanol in a volume ratio of 1:1:1 by weight of the pepper concentrated liquid is added, and stirring extraction is carried out at room temperature for 2-3 hours, then liquid separation is performed to obtain extraction liquid B and waste water; (7) desolventization The extraction liquid A and the extraction liquid B are respectively transferred into an evaporator, and the solvent is removed to obtain finished pepper oleoresin.

2. The process of extracting oleoresin from fresh industrial chilli with low energy and low solvent consumption as claimed in claim 1, wherein, The compound enzyme preparation is composed of pectinase, cellulase and protease in a weight ratio of 1:1:

1.

3. The method of claim 1 or 2, wherein the method of extracting oleoresin from fresh industrial pepper with low energy consumption and low solvent consumption is characterized by, In the step (5) of concentrating the pepper water, the membrane precision of the membrane concentrator is 200 Da.

4. The method for extracting capsicum oleoresin from fresh industrial pepper with low energy consumption and low solvent consumption according to claim 1, characterized in that: The filter residue obtained in the step (4) is subjected to steam stripping to separate residual solvent and dried residue.

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