Method for extracting polyphenols from idesia polycarpa cakes

Abstract

The invention relates to the technical field of polyphenol extraction. The invention provides an extraction method of idesia cake polyphenol, which is characterized by comprising the following steps: (1) crushing and drying idesia cake obtained after pretreatment to obtain idesia cake powder; (2) mixing the idesia cake powder with 30-50% by volume of ethanol, performing ultrasonic treatment, and centrifuging to obtain an idesia cake powder polyphenol solution; and (3) carrying out rotary evaporation on the idesia cake powder polyphenol solution, and concentrating to obtain the idesia cake powder polyphenol. By adopting the process operation and parameter conditions to extract the idesia cake polyphenol, the problems of poor effect, complex components and the like in the idesia cake polyphenol extraction process in the prior art can be effectively solved, and the extraction rate of the polyphenol is remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of polyphenol extraction, and particularly to a method for extracting polyphenols from Idesia polycarpa Maxim. cake and residue. Background Art

[0002] Idesia polycarpa Maxim., also known as oil grape or water wax gourd, is a deciduous tree belonging to the Salicaceae family. It is not only favored for its ornamental and greening value, but also well-known for its rich oil content in fruits and seeds. Moreover, the fruits and seeds of Idesia polycarpa Maxim. also contain a rich content of unsaturated fatty acids, such as linoleic acid, as well as bioactive components such as tocopherol, β-sitosterol, and squalene. Due to the presence of the above-mentioned rich bioactive components, it has health care functions such as enhancing the body's antioxidant and immune capabilities, promoting growth and development, regulating blood cholesterol and triglyceride levels, reducing blood lipid, softening blood vessels, lowering blood pressure, and promoting microcirculation. In addition, the fruits of Idesia polycarpa Maxim. contain rich tryptophan, protein, and various vitamins, so Idesia polycarpa Maxim. is an important edible functional fruit.

[0003] Plant polyphenols are a class of natural compounds widely present in plants, which are composed of one or more aromatic rings combined with one or more hydroxyl groups. These compounds play important roles in plants, including protecting plants from environmental stress and pathogen attacks. In higher plants, thousands of polyphenol molecules have been identified, and they are not only present in inedible parts, but also widely present in edible parts of human daily diet.

[0004] As a valuable natural resource, Idesia polycarpa Maxim. contains rich polyphenolic compounds, which have attracted much attention due to their antioxidant, anti-inflammatory, and potential cardiovascular health benefits. However, the traditional soaking extraction method has shown obvious limitations when dealing with Ephedra sinica Stapf roots. This ancient technique not only takes a long time, but also has low extraction efficiency, resulting in a low content of target components in the final product and often accompanied by a large amount of impurities, seriously restricting its value in pharmacological research and practical applications.

[0005] Therefore, it is particularly urgent to explore and develop a more efficient, fast, and simple method for extracting polyphenols from Idesia polycarpa Maxim. cake and residue, which also has important academic significance and broad market prospects for promoting technological progress and product upgrading in related fields. Summary of the Invention

[0006] The purpose of the present invention is to provide a method for extracting polyphenols from Idesia polycarpa Maxim. cake and residue. By using the process operation and parameter conditions described in the present invention for extracting polyphenols from Idesia polycarpa Maxim. cake and residue, the problems of poor effect and complex components in the existing technology for extracting polyphenols from Idesia polycarpa Maxim. cake and residue can be effectively solved, and the extraction rate of polyphenols can be significantly improved.

[0007] To achieve the above-mentioned invention object, the present invention provides the following technical solutions:

[0008] The present invention provides a method for extracting polyphenols from Idesia polycarpa Maxim. cake meal, comprising the following steps:

[0009] (1) Crushing and drying the Idesia polycarpa Maxim. cake meal obtained after pretreatment to obtain Idesia polycarpa Maxim. cake meal powder;

[0010] (2) Mixing the Idesia polycarpa Maxim. cake meal powder with ethanol having a volume fraction of 30 - 50% and performing ultrasonic treatment, and then centrifuging to obtain an Idesia polycarpa Maxim. cake meal powder polyphenol solution;

[0011] (3) Rotating and evaporating and concentrating the Idesia polycarpa Maxim. cake meal powder polyphenol solution to obtain the product.

[0012] Preferably, in step (1), after crushing, it is sieved through a sieve, and the mesh number of the sieve is 10 - 80 meshes.

[0013] Preferably, in step (2), the material - liquid ratio of the Idesia polycarpa Maxim. cake meal powder to ethanol is 1 g:(15 - 30) mL.

[0014] Preferably, in step (2), the temperature of the ultrasonic treatment is 50 - 70 °C, and the time of the ultrasonic treatment is 20 - 35 min.

[0015] Preferably, in step (2), the rotation speed of the centrifugation is 3000 - 4000 rpm, and the time of the centrifugation is 15 - 30 min.

[0016] Preferably, in step (2), it is concentrated to 20 - 30% of the volume of the Idesia polycarpa Maxim. cake meal powder polyphenol solution.

[0017] By adopting the above - mentioned technical solutions, the present invention has the following beneficial effects:

[0018] In the technical solution of the present invention, the optimized extraction operation and corresponding parameter conditions are adopted. Using the optimized process operation and parameter conditions described in the present invention for extracting polyphenols from Idesia polycarpa Maxim. cake meal can effectively solve the problems of poor effect and complex components in the prior art for the extraction process of polyphenols from Idesia polycarpa Maxim. cake meal, and significantly improve the extraction rate of polyphenols. Moreover, the extraction method described in the present invention is simple and fast to operate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is the standard curve graph of gallic acid as the reference substance. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0020] The present invention provides a method for extracting polyphenols from Idesia polycarpa Maxim. cake meal, comprising the following steps:

[0021] (1) Crushing and drying the Idesia polycarpa Maxim. cake meal obtained after pretreatment to obtain Idesia polycarpa Maxim. cake meal powder;

[0022] (2) Mix the Idesia polycarpa Maxim. cake meal powder with ethanol at a volume fraction of 30 - 50%, and then perform ultrasonic treatment. After centrifugation, obtain the polyphenol solution of the Idesia polycarpa Maxim. cake meal powder;

[0023] (3) Rotate evaporate and concentrate the polyphenol solution of the Idesia polycarpa Maxim. cake meal powder to obtain the product.

[0024] In the present invention, after cleaning, drying, and removing the roots and stems of fresh Idesia polycarpa Maxim. fruits, perform pressing treatment to obtain the Idesia polycarpa Maxim. cake meal.

[0025] In the present invention, the temperature of the drying treatment is preferably 50 - 70°C, more preferably 55 - 65°C, and even more preferably 65°C; the time of the drying treatment is preferably 24 - 72 h, more preferably 36 - 60 h, and even more preferably 48 h; the pressing method is preferably the cold pressing method.

[0026] In the present invention, then crush and dry the obtained Idesia polycarpa Maxim. cake meal to obtain the Idesia polycarpa Maxim. cake meal powder. In the present invention, after the Idesia polycarpa Maxim. cake meal is crushed, it is sieved through a sieve, and the material passing through the sieve is collected. The mesh number of the sieve is preferably 10 - 80 meshes, more preferably 30 - 50 meshes, and even more preferably 40 meshes. Then perform drying treatment on the collected material passing through the sieve. The drying temperature is preferably 50 - 70°C, more preferably 55 - 68°C, and even more preferably 65°C; the drying time is preferably 24 - 72 h, more preferably 36 - 60 h, and even more preferably 48 h.

[0027] In the present invention, mix the obtained Idesia polycarpa Maxim. cake meal powder with ethanol for ultrasonic treatment. The volume fraction of the ethanol is preferably 30 - 50%, more preferably 35 - 45%, and even more preferably 40%. The material - liquid ratio of the Idesia polycarpa Maxim. cake meal powder to ethanol is preferably 1 g:(15 - 30) mL, more preferably 1 g:(18 - 25) mL, and even more preferably 1 g:20 mL. The power of the ultrasonic treatment in the present invention is preferably 240 - 400 W, more preferably 280 - 360 W, and even more preferably 300 W; the temperature of the ultrasonic treatment is preferably 50 - 70°C, more preferably 55 - 65°C, and even more preferably 60°C; the time of the ultrasonic treatment is preferably 20 - 35 min, more preferably 22 - 30 min, and even more preferably 25 min; the number of times of the ultrasonic treatment is preferably 1 - 3 times, and more preferably 2 times.

[0028] In the present invention, after ultrasonic treatment, centrifugation is carried out to separate the solid from the liquid, and the supernatant is collected to obtain the polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder. The rotation speed of the centrifugation in the present invention is preferably 3000 - 4000 rpm, more preferably 3200 - 3800 rpm, and even more preferably 3500 rpm; the time of the centrifugation is preferably 15 - 30 min, more preferably 18 - 25 min, and even more preferably 20 min.

[0029] In the present invention, the obtained polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder is subjected to rotary evaporation. The temperature of the rotary evaporation is preferably 40 - 70 °C, more preferably 45 - 65 °C, and even more preferably 60 °C. The present invention preferably concentrates it to 20 - 30% of the volume of the polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder, more preferably 22 - 28%, and even more preferably 25%.

[0030] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0031] Example 1

[0032] A method for extracting polyphenols from Idesia polycarpa Maxim. cake and meal comprises the following steps:

[0033] (1) Wash the fresh Idesia polycarpa Maxim. fruits, then dry them at 65 °C for 48 h. After removing the rhizomes, cold pressing is used to extract oil to obtain the Idesia polycarpa Maxim. cake and meal;

[0034] (2) After crushing the Idesia polycarpa Maxim. cake and meal, pass it through a 40 - mesh sieve, collect the material under the sieve and dry it at 65 °C for 24 h to obtain the Idesia polycarpa Maxim. cake and meal powder;

[0035] (3) Mix the Idesia polycarpa Maxim. cake and meal powder with 40% ethanol at a ratio of 1 g:15 mL, then carry out ultrasonic treatment at 60 °C and 300 W for 30 min, and then centrifuge at 3500 rpm for 20 min to separate the solid from the liquid, and collect the supernatant to obtain the polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder;

[0036] (4) Carry out rotary evaporation on the polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder at 60 °C, and concentrate it to 25% of the volume of the polyphenol solution of the Idesia polycarpa Maxim. cake and meal powder to obtain the crude Idesia polycarpa Maxim. polyphenols.

[0037] Example 2

[0038] A method for extracting polyphenols from Idesia polycarpa Maxim. cake and meal comprises the following steps:

[0039] (1) Wash the fresh Idesia polycarpa Maxim. fruits, then dry them at 65 °C for 48 h. After removing the rhizomes, cold pressing is used to extract oil to obtain the Idesia polycarpa Maxim. cake and meal;

[0040] (2) After the ash cake is crushed, it is passed through a 40-mesh sieve, and the sieved material is collected and dried at 65° C. for 24 hours to obtain ash cake powder;

[0041] (3) Mixing the Alpinia schrenkiana cake powder with 40% ethanol at a ratio of 1 g: 20 mL, and then ultrasonically treating it at 70°C and 300 W for 25 min, and then centrifuging it at 3500 rpm for 20 min to separate the solid and liquid, and collecting the supernatant to obtain the Alpinia schrenkiana cake powder polyphenol solution;

[0042] (4) The polyphenol solution of the ash tree seed cake powder was concentrated by rotary evaporation at 60° C. to 25% of the volume of the polyphenol solution of the ash tree seed cake powder, thereby obtaining a crude product of ash tree seed polyphenol.

[0043] Example 3

[0044] A method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0045] (1) The fresh ash fruit was cleaned, dried at 65°C for 48 hours, and the rhizomes were removed, and the oil was extracted by cold pressing to obtain ash cake;

[0046] (2) After the ash cake is crushed, it is passed through a 40-mesh sieve, and the sieved material is collected and dried at 65° C. for 24 hours to obtain ash cake powder;

[0047] (3) Mixing the ash cake powder with 40% ethanol at a ratio of 1 g: 20 mL, and then ultrasonically treating it at 60°C and 300 W for 25 min, and then centrifuging it at 3500 rpm for 20 min to separate the solid and liquid, and collecting the supernatant to obtain the ash cake powder polyphenol solution;

[0048] (4) The polyphenol solution of the ash tree seed cake powder was concentrated by rotary evaporation at 60° C. to 25% of the volume of the polyphenol solution of the ash tree seed cake powder, thereby obtaining a crude product of ash tree seed polyphenol.

[0049] Example 4

[0050] A method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0051] (1) The fresh ash fruit was cleaned, dried at 65°C for 48 hours, and the rhizomes were removed, and the oil was extracted by cold pressing to obtain ash cake;

[0052] (2) After the ash cake is crushed, it is passed through a 40-mesh sieve, and the sieved material is collected and dried at 65° C. for 24 hours to obtain ash cake powder;

[0053] (3) Mix the Idesia polycarpa Maxim. cake meal powder with 40% ethanol at a ratio of 1 g: 20 mL, then perform ultrasonic treatment at 70 °C and 300 W for 35 min, and then centrifuge at 3500 rpm for 20 min for solid-liquid separation. Collect the supernatant to obtain the Idesia polycarpa Maxim. cake meal powder polyphenol solution;

[0054] (4) Rotate and evaporate the Idesia polycarpa Maxim. cake meal powder polyphenol solution at 60 °C, and concentrate it to 25% of the volume of the Idesia polycarpa Maxim. cake meal powder polyphenol solution to obtain the crude Idesia polycarpa Maxim. polyphenol.

[0055] Example 5

[0056] A method for extracting Idesia polycarpa Maxim. cake meal polyphenol, the steps are as follows:

[0057] (1) Wash the fresh Idesia polycarpa Maxim. fruits, then dry them at 65 °C for 48 h. After removing the roots and rhizomes, use the cold pressing method to extract oil to obtain the Idesia polycarpa Maxim. cake meal;

[0058] (2) After crushing the Idesia polycarpa Maxim. cake meal, pass it through a 40-mesh sieve, collect the material under the sieve and dry it at 65 °C for 24 h to obtain the Idesia polycarpa Maxim. cake meal powder;

[0059] (3) Mix the Idesia polycarpa Maxim. cake meal powder with 40% ethanol at a ratio of 1 g: 30 mL, then perform ultrasonic treatment at 60 °C and 300 W for 35 min, and then centrifuge at 3500 rpm for 20 min for solid-liquid separation. Collect the supernatant to obtain the Idesia polycarpa Maxim. cake meal powder polyphenol solution;

[0060] (4) Rotate and evaporate the Idesia polycarpa Maxim. cake meal powder polyphenol solution at 60 °C, and concentrate it to 25% of the volume of the Idesia polycarpa Maxim. cake meal powder polyphenol solution to obtain the crude Idesia polycarpa Maxim. polyphenol.

[0061] Comparative Example 1

[0062] Same as Example 1, only replace the ethanol concentration with 60%.

[0063] Comparative Example 2

[0064] Same as Example 5, only replace the material-liquid ratio with 1 g: 35 mL.

[0065] Comparative Example 3

[0066] Same as Example 1, only replace the ethanol concentration with 70%.

[0067] Test Example 1

[0068] (I) Draw the standard curve

[0069] Prepare a standard solution of gallic acid reference substance at a concentration of 1 mg / mL. Take 1 mL of reference substance solutions with concentrations of 10, 20, 30, 40, and 50 μg / mL respectively and place them in 25-mL colorimetric tubes. Add 1 mL of 0.1 mol / L Folin-Ciocalteu reagent solution and 4 mL of 7.5% sodium carbonate solution. After mixing, make up the volume to the mark with pure water. Keep it in the dark for 1 hour for color development, and record the absorbance of the solution at 765 nm.

[0070] Measure the absorbance value at 765 nm. Use the absorbance value A as the ordinate and the mass concentration of gallic acid as the abscissa to plot the standard curve of gallic acid, and obtain the linear regression equation y = 0.0046x - 0.0013R 2 = 0.9992. (II)

[0072] Determine the extraction rates of the polyphenols from the Idesia polycarpa Maxim. cake and meal extracted in Examples 1 - 5 and Comparative Examples 1 - 3. Using the Folin-Ciocalteu method, take 1 mL of the polyphenol extract from the Idesia polycarpa Maxim. cake and meal and dilute it to 10 mL. Take 1 mL and place it in a 25-mL colorimetric tube. Add 1 mL of 0.1 mol / L Folin-Ciocalteu reagent solution and 4 mL of 7.5% sodium carbonate solution. After mixing, make up the volume to the mark with pure water and keep it in the dark for 1 h.

[0073] Measure the corresponding absorbance at a wavelength of 765 nm, and substitute the measured absorbance into the above-mentioned gallic acid standard curve. Calculate the polyphenol content (mg / g) according to the standard curve.

[0074]

[0075] In the formula, C is the polyphenol mass concentration obtained from the standard curve, μg / mL; N is the sample dilution factor, V is the volume after the extraction solution is made up to the mark, mL; M is the mass of the Idesia polycarpa Maxim. cake and meal powder, g.

[0076] Table 1 Extraction rate of polyphenols from the Idesia polycarpa Maxim. cake and meal in Examples 1 - 5 and Comparative Examples 1 - 3

[0077]

[0078]

[0079] By comparing the data of Examples 1 - 5 and Comparative Examples 1 - 3, it is found that the extraction rate of the polyphenols from the Idesia polycarpa Maxim. cake and meal prepared in the examples is significantly higher than that in the comparative examples. It also shows that ultrasonic time, ultrasonic temperature, ethanol concentration, and solid-liquid ratio all have obvious effects on the extraction of polyphenols from the Idesia polycarpa Maxim. cake and meal.

[0080] In summary, it can be seen that by adopting the optimized process operation and parameter conditions described in the present invention for the extraction of polyphenols from Idesia polycarpa Maxim. cake and meal, the problem of poor effect in the existing polyphenol extraction process from Idesia polycarpa Maxim. cake and meal can be effectively solved, and the extraction rate of polyphenols can be significantly improved.

[0081] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A method for extracting polyphenols from Idesia polycarpa Maxim. cake residue, characterized in that, It includes the following steps: (1) Crush and dry the processed Idesia polycarpa Maxim cake residue to obtain Idesia polycarpa Maxim cake residue powder; (2) Mix the Idesia polycarpa Maxim cake residue powder with ethanol with a volume fraction of 30 - 50% and perform ultrasonic treatment, then centrifuge to obtain the polyphenol solution of Idesia polycarpa Maxim cake residue powder; (3) Rotate and evaporate and concentrate the polyphenol solution of Idesia polycarpa Maxim cake residue powder to obtain the product.

2. The extraction method according to claim 1, characterized in that, After the crushing in step (1), it is sieved through a sieve, and the mesh number of the sieve is 10 - 80 meshes.

3. The extraction method according to claim 1, wherein The material-liquid ratio of the Idesia polycarpa Maxim cake residue powder and ethanol in step (2) is 1 g:(15 - 30) mL.

4. The extraction method according to claim 1, wherein The temperature of the ultrasonic treatment in step (2) is 50 - 70 °C, and the time of the ultrasonic treatment is 20 - 35 min.

5. The extraction method according to claim 1, wherein The rotation speed of the centrifuge in step (2) is 3000 - 4000 rpm, and the time of the centrifuge is 15 - 30 min.

6. The extraction method according to claim 1, characterized in that, Concentrate to 20 - 30% of the volume of the polyphenol solution of Idesia polycarpa Maxim cake residue powder in step (2).

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