Method for extracting antioxidant component from pineapple peel
Through ultrasonic-assisted ethanol extraction method, the antioxidant components in pineapple skin are extracted, solving the problem of unused pineapple skin resources and achieving efficient, environmentally friendly and economical extraction effects.
Patent Information
- Application Number
- CN202410400036.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-03
- Publication Date
- 2025-03-18
AI Technical Summary
The pineapple peel resources are not effectively utilized, resulting in resource waste and environmental pollution. At the same time, traditional extraction methods have problems such as high cost, multi-solvent use and low extraction rates.
Ultrasonic assisted ethanol extraction method was used to mix pineapple skin powder with 50% ethanol, sonicate, then filter and concentrate under reduced pressure, and finally the antioxidant components were extracted by freeze-drying.
It improves the extraction rate of antioxidant components in pineapple skin, reduces solvent use and cost, simplifies the process flow, and converts waste into valuable products, with environmental and economic advantages.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of plant natural component extraction, and specifically relates to a method for extracting antioxidant components from pineapple peel. Background Art
[0002] Pineapple belongs to the genus Anineapple of the Bromeliaceae family. my country has abundant pineapple resources and produces a large amount of pineapple waste every year. The highest proportion of pineapple waste is pineapple peel, accounting for about 30-40%. The various usable ingredients contained in it have not been recycled, which not only wastes a lot of resources, but also pollutes the ecological environment of the processing area. Pineapple peel has similar nutritional components to pineapple flesh, including sugars, vitamins, carotenoids and minerals. It also contains flavonoids, polyphenols and protein substances with antioxidant properties. Antioxidant compounds play an important role in inhibiting and delaying lipid oxidation or any other biological molecules. They are also beneficial to metabolism. It is of great significance to health, cosmetics and chemical industries.
[0003] Ultrasonic-assisted ethanol extraction method promotes the formation of cavitation bubbles through ultrasound. The bubbles can pass through the cell wall of the plant matrix, which is beneficial to the contact between the solvent and the extract, thereby reducing the extraction time and improving the yield and quality. Compared with other extraction processes, it has higher extraction rate, limited solvent use, lower cost, and is more environmentally friendly and green, and these advantages can solve the limitations brought by traditional methods. The present invention improves the comprehensive utilization of pineapple waste by converting waste into valuable products, and has a positive impact on the economy and the environment. Summary of the invention
[0004] The purpose of the present invention is to provide a method for extracting antioxidant components from pineapple peel, so as to realize the conversion of waste into valuable products, increase the value of waste, simplify the extraction process, reduce the use of harmful and expensive solvents, and improve the extraction rate.
[0005] In order to achieve the above-mentioned invention object, the present invention provides the following technical solutions:
[0006] (1) washing pineapple peel with tap water, drying to constant weight at a constant temperature of 40° C., crushing and sieving to obtain pineapple peel powder;
[0007] (2) weighing pineapple peel powder and mixing it with an extraction solvent in proportion, and performing ultrasonic treatment to obtain residue and supernatant;
[0008] (3) filtering the supernatant to remove the residue and extracting the antioxidant components;
[0009] (4) The antioxidant component extract is concentrated under reduced pressure and freeze-dried to obtain the antioxidant components in the pineapple peel.
[0010] Preferably, the extracted antioxidant components are flavonoids, polyphenols, and proteins.
[0011] Preferably, the extraction solvent in step (2) is 50% ethanol, the solid-liquid ratio of pineapple peel powder to the extraction solvent is 1:10-1:30 (g / mL), the ultrasonic time is 30-150 min, the ultrasonic temperature is 30-70° C., and the ultrasonic power is 120-360 W.
[0012] Preferably, the filtration in step (3) uses filter paper with a pore size of 15-20 microns.
[0013] Preferably, step (4) is carried out at 40°C under reduced pressure.
[0014] Further preferably, when the extracted antioxidant component is flavonoids, the solid-liquid ratio of pineapple peel powder to extraction solvent is 1:10 g / mL, the ultrasonic time is 60 min, the ultrasonic temperature is 50° C., and the ultrasonic power is 240 W.
[0015] Further preferably, when the extracted antioxidant component is polyphenol, the solid-liquid ratio of pineapple peel powder to extraction solvent is 1:10 g / mL, the ultrasonic time is 30 min, the ultrasonic temperature is 40° C., and the ultrasonic power is 240 W.
[0016] Further preferably, when the extracted antioxidant component is protein, the solid-liquid ratio of pineapple peel powder to extraction solvent is 1:10 g / mL, the ultrasonic time is 60 min, the ultrasonic temperature is 50° C., and the ultrasonic power is 180 W.
[0017] Beneficial effects of the present invention: The present invention provides a method for extracting antioxidant components from pineapple peel, including flavonoids, polyphenols, and proteins, and takes the content in the extract as the measured value to provide optimized process conditions. Nowadays, pineapple peel is less utilized. The antioxidant components extracted by the present invention can be added to baked foods as antioxidants, providing a method for the comprehensive utilization of pineapple peel. The extraction method uses safe and environmentally friendly antioxidant ethanol, assisted by ultrasound, limited solvent use, lower cost, and simpler operation. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 This is the effect of the solid-liquid ratio on the total flavonoids content of the extract.
[0019] Figure 2 The effect of ultrasonic time on the total flavonoids content of the extract.
[0020] Figure 3 The effect of ultrasonic temperature on the total flavonoids content of the extract.
[0021] Figure 4 The effect of ultrasonic power on the total flavonoids content of the extract.
[0022] Figure 5 This is the effect of the solid-liquid ratio on the total polyphenol content of the extract.
[0023] Figure 6 The effect of ultrasonic time on the total polyphenol content of the extract.
[0024] Figure 7 The effect of ultrasonic temperature on the total polyphenol content of the extract.
[0025] Figure 8 The effect of ultrasonic power on the total polyphenol content of the extract.
[0026] Fig. 9 This is the effect of the solid-liquid ratio on the total protein content of the extract.
[0027] Fig.10 The effect of ultrasonic time on the total protein content of the extract.
[0028] Fig.11 The effect of ultrasonic temperature on the total protein content of the extract.
[0029] Fig.12 The effect of ultrasonic power on the total protein content of the extract. DETAILED DESCRIPTION
[0030] The present invention is further described in detail below with reference to the accompanying drawings and embodiments.
[0031] Example 1
[0032] Weigh an appropriate amount of processed pineapple peel powder, mix it with 50% ethanol, and extract it under the conditions of ultrasonic time 30 min, ultrasonic temperature 50°C, ultrasonic power 240 W, and solid-liquid ratios of 1:10 g / mL, 1:15 g / mL, 1:20 g / mL, 1:25 g / mL, and 1:30 g / mL, respectively, to obtain a supernatant and a residue, and filter the supernatant with filter paper to obtain an extract.
[0033] Experimental Example 2
[0034] Weigh an appropriate amount of processed pineapple peel powder, mix it with 50% ethanol, and extract it under the conditions of a solid-liquid ratio of 1:10 g / mL, an ultrasonic temperature of 50° C., an ultrasonic power of 240 W, and ultrasonic times of 30 min, 60 min, 90 min, 120 min, and 150 min, respectively, to obtain a supernatant and a filter residue, and filter the supernatant with filter paper to obtain an extract.
[0035] Experimental Example 3
[0036] Weigh an appropriate amount of processed pineapple peel powder, mix it with 50% ethanol, extract under the conditions of a solid-liquid ratio of 1:10 g / mL, ultrasonic time of 30 min, ultrasonic power of 240 W, and ultrasonic temperatures of 30° C., 40° C., 50° C., 60° C., and 70° C., respectively, to obtain a supernatant and a filter residue, and filter the supernatant with filter paper to obtain an extract.
[0037] Experimental Example 4
[0038] Weigh an appropriate amount of processed pineapple peel powder, mix it with 50% ethanol, and extract it under the conditions of a solid-liquid ratio of 1:10 g / mL, an ultrasonic time of 30 min, an ultrasonic temperature of 50° C., and ultrasonic powers of 120 W, 150 W, 180 W, 240 W, and 300 W, respectively, to obtain a supernatant and a filter residue, and filter the supernatant with filter paper to obtain an extract.
[0039] Experimental Example 5
[0040] An appropriate amount of processed pineapple peel powder is weighed, mixed with 50% ethanol, extracted under the conditions of a solid-liquid ratio of 1:10 g / mL, an ultrasonic time of 60 min, an ultrasonic temperature of 50° C., and an ultrasonic power of 240 W to obtain a supernatant and a filter residue, and the supernatant is filtered with filter paper to obtain an extract. The extract is concentrated under reduced pressure and freeze-dried to obtain flavonoids.
[0041] Experimental Example 6
[0042] An appropriate amount of processed pineapple peel powder is weighed, mixed with 50% ethanol, extracted under the conditions of a solid-liquid ratio of 1:10 g / mL, an ultrasonic time of 30 min, an ultrasonic temperature of 40° C., and an ultrasonic power of 240 W to obtain a supernatant and a filter residue, and the supernatant is filtered with filter paper to obtain an extract. The extract is concentrated under reduced pressure and freeze-dried to obtain polyphenols.
[0043] Experimental Example 7
[0044] An appropriate amount of processed pineapple peel powder is weighed, mixed with 50% ethanol, extracted under the conditions of a solid-liquid ratio of 1:10 g / mL, an ultrasonic time of 60 min, an ultrasonic temperature of 50° C., and an ultrasonic power of 120 W to obtain a supernatant and a filter residue, and the supernatant is filtered with filter paper to obtain an extract. The extract is concentrated under reduced pressure and freeze-dried to obtain protein.
[0045] Comparative experiment
[0046] Comparative Example 1
[0047] Flavonoid content determination: Sodium nitrite-aluminum nitrate method was used, catechin was used as standard, standard curve was drawn, absorbance value was measured at 510 nm, and mass concentration of flavonoids in the extract was calculated according to the standard curve.
[0048] Flavonoid content (mg / g) = C1V1 / M1;
[0049] Where:
[0050] C1: flavonoid mass concentration mg / mL;
[0051] V1: total volume of the extract, mL;
[0052] M1: The mass of the weighed pineapple peel powder in g.
[0053] like Figure 1 As shown in the figure, the flavonoid content in the extract increases with the increase of the solid-liquid ratio and then decreases. At 1:25 g / mL, it reaches a maximum of 1.92 mg / g and then decreases slightly. Figure 2 As shown in the figure, the flavonoid content increases with time and then decreases. The best extraction effect is 1.99 mg / g at 60 minutes. After more than 60 minutes, the content decreases. Figure 3 As shown in the figure, the flavonoid content first increases with the temperature, reaching 1.85 mg / g at 50°C, and then decreases slightly with fluctuations. Figure 4 As shown, the flavonoid content reached 1.87 mg / g when the ultrasonic power increased to 240 W, and further increasing the ultrasonic power had little effect on the flavonoid content.
[0054] Comparative Example 2
[0055] Determination of polyphenol content: The Folin-phenol method was used, with gallic acid as the standard, a standard curve was drawn, the absorbance value was measured at 750 nm, and the mass concentration of polyphenols in the extract was calculated based on the standard curve.
[0056] Polyphenol content (mg / g) = C2V2 / M2;
[0057] Where:
[0058] C2: polyphenol mass concentration mg / mL;
[0059] V2: total volume of the extract, mL;
[0060] M2: The mass of the weighed pineapple peel powder in g.
[0061] like Figure 5 As shown in the figure, the polyphenol content in the extract increases with the increase of the solid-liquid ratio. When it reaches 1:20 g / mL, the polyphenol content changes little when the solid-liquid ratio continues to increase. Figure 6 As shown in the figure, with the increase of ultrasonic time, the polyphenol content gradually decreased, and the highest value was 7.39 mg / g at 30 min in the range of 30 min to 150 min. Figure 7As shown in the figure, the polyphenol content increases first and then decreases with the increase of temperature, and the highest content is 7.48 mg / g when the temperature reaches 40°C. Figure 8 As shown, with the increase of power, the polyphenol content first increased to reach a maximum of 7.09 mg / g at 240 W, and then decreased.
[0062] Comparative Example 3
[0063] Protein content determination: The Coomassie brilliant blue method was used, with bovine serum albumin as the standard, a standard curve was drawn, the absorbance value was measured at 595 nm, and the protein mass concentration in the extract was calculated based on the standard curve.
[0064] Protein content (mg / g) = C3V3 / M3;
[0065] Where:
[0066] C3: protein concentration mg / mL;
[0067] V3: total volume of the extract, mL;
[0068] M3: The mass of the weighed pineapple peel powder in g.
[0069] like Fig. 9 As shown in the figure, the protein content of the extract first increases and then decreases with the increase of the material-liquid ratio, and the highest content is 18.29 mg / g when it reaches 1:20 g / mL. Fig.10 As shown in the figure, with the increase of time, the protein content first increased and reached a maximum of 21.23 mg / g at 60 min, and then decreased. Fig.11 As shown in the figure, when the temperature is between 30℃ and 50℃, the protein content increases, reaching the highest level at 50℃, with a content of 18.42 mg / g. As the temperature continues to increase, the protein content decreases. Fig.12 As shown, the protein content first increased and then decreased with the increase of ultrasonic power, reaching a maximum of 18.13 mg / g when the power was 180 W.
[0070] Comparative Example 4
[0071] Determination of DPPH free radical scavenging ability: Take 1 mL of the solution prepared by the antioxidant components obtained in Example 5, Example 6 and Example 7, add 3 mL of DPPH solution, this is used as the sample group; take 1 mL of anhydrous ethanol, then add 3 mL of DPPH solution, as the blank group; take 1 mL of 1 mg / mL antioxidant component solution, then add 3 mL of anhydrous ethanol, as the control group. c As a positive control, keep the sample away from light for 30 minutes and measure the absorbance at 517 nm.
[0072] Calculation method of clearance rate: Clearance rate % = [1-(A1-A2) / A0] × 100;
[0073] Where:
[0074] A0 = absorbance of blank group;
[0075] A1 = sample group absorbance;
[0076] A2 = absorbance of control group.
[0077] The results were as follows: 0.2 mg / mL flavonoid solution, polyphenol solution, protein solution, V c The solution clearance rates were 74.32%, 82.61%, 59.79% and 79.55% respectively.
[0078] Comparative Example 5
[0079] Determination of ABTS free radical scavenging ability: Take 0.6 mL of the solution prepared by the antioxidant components obtained in Example 5, Example 6 and Example 7, add 1.6 mL of ABTS solution, and this is used as the sample group; take 0.6 mL of anhydrous ethanol, and then add 1.6 mL of ABTS solution, and this is used as the blank group. c As a positive control, keep the sample away from light for 5 minutes and measure the absorbance at 734 nm.
[0080] Calculation method of clearance rate: Clearance rate % = [1-(A1-A2) / A0] × 100;
[0081] Where:
[0082] A0 = absorbance of blank group;
[0083] A1 = sample group absorbance;
[0084] A2 = absorbance of control group.
[0085] The results were as follows: 0.2 mg / mL flavonoid solution, polyphenol solution, protein solution, V c The solution clearance rates were 57.14%, 40.52%, 51.29% and 70.12% respectively.
[0086] The above embodiments have provided a very specific and detailed description of the implementation methods of the present invention, which is not a limitation of the present invention. Any modifications, equivalent substitutions and improvements based on the present invention that do not deviate from the technical solution of the present invention should be included in the protection scope of the patent of the present invention.
Claims
1. A process for extracting antioxidant active ingredients from pineapple peel, comprising the following steps: (1) washing pineapple peel with tap water, drying to constant weight at a constant temperature of 40° C., crushing and sieving to obtain pineapple peel powder; (2) weighing pineapple peel powder and mixing it with an extraction solvent in proportion, and performing ultrasonic treatment to obtain residue and supernatant; (3) filtering the supernatant to remove residues to obtain an antioxidant component extract; (4) The antioxidant component extract is concentrated under reduced pressure and freeze-dried to obtain the antioxidant components in the pineapple peel.
2. The extraction method according to claim 1, characterized in that: The antioxidant active ingredients are flavonoids, polyphenols and proteins.
3. The extraction method according to claim 1, characterized in that The pineapple peel powder after crushing in step (1) needs to be sieved through a 60-mesh sieve.
4. The extraction method according to claim 1, characterized in that In step (2), the extraction solvent is 50% ethanol, the solid-liquid ratio is 1:10-1:30 (g / ml), the ultrasonic time is 30-150 minutes, the ultrasonic temperature is 30-70° C., and the ultrasonic power is 120-360W.
5. The extraction method according to claim 1, characterized in that In step (3), the filtration is performed using filter paper with a pore size of 15-20 microns.
6. The extraction method according to claim 1, characterized in that In step (4), the reaction mixture is concentrated under reduced pressure at 40°C.