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 invention relates to the technical field of polyphenol extraction, and in particular to a method for extracting polyphenol from Castanopsis schrenkiana cake. Background Art

[0002] Castanopsis altissima, also known as oil grape or water melon, is a deciduous tree belonging to the family Salicaceae. It is not only favored for its ornamental and greening value, but also famous for its rich oil content in its fruits and seeds. Moreover, Castanopsis altissima fruits and seeds are also rich in unsaturated fatty acids, such as linoleic acid, as well as bioactive ingredients such as tocopherol, β-sitosterol and squalene. Due to its rich bioactive ingredients, it has health benefits such as enhancing the body's antioxidant and immune capabilities, promoting growth and development, regulating blood cholesterol and triglyceride levels, lowering blood lipids, softening blood vessels, lowering blood pressure, and promoting microcirculation. In addition, Castanopsis altissima fruit is rich in tryptophan, protein and multiple vitamins, so Castanopsis altissima is an important edible functional fruit.

[0003] Plant polyphenols are a class of natural compounds widely found in plants. They 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 pathogens. In higher plants, thousands of polyphenol molecules have been identified, which are not only present in inedible parts, but also widely found in edible parts of human daily diet.

[0004] As a valuable natural resource, Ephedra sinica contains rich polyphenolic compounds, which have attracted much attention for their antioxidant, anti-inflammatory and potential cardiovascular health benefits. However, the traditional soaking extraction method has exposed obvious limitations when processing Ephedra sinica roots. This ancient technology is not only time-consuming, but also has low extraction efficiency, resulting in low content of target components in the final product and often accompanied by a large amount of impurities, which seriously restricts its value in pharmacological research and practical applications.

[0005] Therefore, it is particularly urgent to explore and develop a more efficient, quick and simple method for extracting polyphenols from Castanopsis orientalis cake, 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 object of the present invention is to provide a method for extracting polyphenols from Castanopsis schrenkiana cake. The process operation and parameter conditions of the present invention are used to extract polyphenols from Castanopsis schrenkiana cake, which can effectively solve the problems of poor effect and complex components in the Castanopsis schrenkiana cake polyphenol extraction process in the prior art, and significantly improve the extraction rate of polyphenols.

[0007] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0008] The present invention provides a method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0009] (1) crushing and drying the tung oil tree cake obtained after the pretreatment to obtain tung oil tree cake powder;

[0010] (2) mixing the Alpinia schrenkiana cake powder with 30-50% by volume ethanol, ultrasonically treating the mixture, and centrifuging the mixture to obtain an Alpinia schrenkiana cake powder polyphenol solution;

[0011] (3) The polyphenol solution of the Castanopsis schrenkiana cake powder is rotary evaporated and concentrated to obtain the polyphenol solution.

[0012] Preferably, the powder is sieved after the pulverization in step (1), and the mesh size of the sieve is 10-80 meshes.

[0013] Preferably, in step (2), the solid-liquid ratio of the mixture of the Castanopsis schrenkiana cake powder and ethanol is 1 g: (15-30) mL.

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

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

[0016] Preferably, the concentration in step (2) is to 20-30% of the volume of the polyphenol solution of Castanopsis schrenkiana cake powder.

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

[0018] The optimized extraction operation and corresponding parameter conditions in the technical solution of the present invention can effectively solve the problems of poor effect and complex components in the prior art of extracting polyphenols from tung oil seed cakes and dregs, and significantly improve the extraction rate of polyphenols. Moreover, the extraction method of the present invention is simple and quick to operate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is the standard curve of the reference substance gallic acid. DETAILED DESCRIPTION

[0020] The present invention provides a method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0021] (1) crushing and drying the tung oil tree cake obtained after the pretreatment to obtain tung oil tree cake powder;

[0022] (2) mixing the Alpinia schrenkiana cake powder with 30-50% by volume ethanol, ultrasonically treating the mixture, and centrifuging the mixture to obtain an Alpinia schrenkiana cake powder polyphenol solution;

[0023] (3) The polyphenol solution of the Castanopsis schrenkiana cake powder is rotary evaporated and concentrated to obtain the polyphenol solution.

[0024] In the present invention, fresh Alpinia schrenkiana fruits are cleaned, dried, and their rhizomes are removed, and then pressed to obtain Alpinia schrenkiana cake.

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

[0026] In the present invention, the obtained ashwagandha cake is then crushed and dried to obtain ashwagandha cake powder. The ashwagandha cake in the present invention is crushed and passed through a sieve, and the sieve underflow is collected. The mesh number of the sieve is preferably 10-80 mesh, more preferably 30-50 mesh, and more preferably 40 mesh. The collected sieve underflow is then dried, and the drying temperature is preferably 50-70°C, more preferably 55-68°C, and more preferably 65°C; the drying time is preferably 24-72h, more preferably 36-60h, and more preferably 48h.

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

[0028] In the present invention, the ultrasonic treatment is followed by centrifugation to separate the solid and the liquid, and the supernatant is collected to obtain the polyphenol solution of the tung oil tree seed cake powder. The centrifugal speed of the present invention is preferably 3000-4000 rpm, more preferably 3200-3800 rpm, and more preferably 3500 rpm; the centrifugal time is preferably 15-30 min, more preferably 18-25 min, and more preferably 20 min.

[0029] In the present invention, the obtained Alpinia schrenkiana cake powder polyphenol solution is subjected to rotary evaporation, and the rotary evaporation temperature is preferably 40-70° C., further preferably 45-65° C., and further preferably 60° C. In the present invention, the polyphenol solution of Alpinia schrenkiana cake powder is preferably concentrated to 20-30% of the volume of the polyphenol solution, further preferably 22-28%, and further 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 tung oil seed cake, comprising the following steps:

[0033] (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;

[0034] (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;

[0035] (3) Mixing the ash cake powder with 40% ethanol at a ratio of 1 g:15 mL, and then ultrasonically treating it at 60°C and 300 W for 30 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;

[0036] (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.

[0037] Example 2

[0038] A method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0039] (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;

[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) 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 35 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;

[0054] (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.

[0055] Example 5

[0056] A method for extracting polyphenols from tung oil seed cake, comprising the following steps:

[0057] (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;

[0058] (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;

[0059] (3) Mixing the ash cake powder with 40% ethanol at a ratio of 1 g:30 mL, and then ultrasonically treating it at 60°C and 300 W for 35 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;

[0060] (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.

[0061] Comparative Example 1

[0062] The same as Example 1, except that the ethanol concentration was changed to 60%.

[0063] Comparative Example 2

[0064] Same as Example 5, except that the solid-liquid ratio was changed to 1 g:35 mL.

[0065] Comparative Example 3

[0066] The same as Example 1, except that the ethanol concentration was changed to 70%.

[0067] Test Example 1

[0068] (I) Drawing a standard curve

[0069] Prepare the reference substance gallic acid into a 1 mg / mL standard solution, take 1 mL of the reference substance solution with a concentration of 10, 20, 30, 40, and 50 μg / mL and place it in a 25 mL colorimetric tube, add 1 mL of 0.1 mol / L folin phenol solution and 4 mL of 7.5% sodium carbonate solution, mix well and make up to volume with pure water, place in the dark for 1 hour to develop color, and record the absorbance of the solution at 765 nm.

[0070] The absorbance value was measured at 765 nm, and the gallic acid standard curve was plotted with the absorbance value A as the ordinate and the mass concentration of gallic acid as the abscissa, and the linear regression equation y = 0.0046x-0.0013R was obtained. 2 =0.9992. (two)

[0072] The extraction rate of polyphenols extracted from the ashwagandha seed cakes in Examples 1-5 and Comparative Examples 1-3 was determined. Using the Folin phenol method, 1 mL of the ashwagandha seed cake polyphenol extract was diluted to 10 mL, 1 mL was placed in a 25 mL colorimetric tube, 1 mL of 0.1 mol / L Folin phenol solution and 4 mL of 7.5% sodium carbonate solution were added, mixed, and then made up to volume with pure water, and protected from light for 1 hour.

[0073] The corresponding absorbance was measured at a wavelength of 765 nm, and the measured absorbance was substituted into the above gallic acid standard curve to calculate the polyphenol content (mg / g) according to the standard curve.

[0074]

[0075] Wherein, C is the mass concentration of polyphenols obtained from the standard curve, μg / mL; N is the sample dilution multiple, V is the volume of the extract after constant volume, mL; M is the mass of the Castanopsis altissima cake powder, g.

[0076] Table 1 Extraction rate of polyphenols from tung oil seed cake of 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 polyphenols from the tung oilseed cake prepared in the Examples is significantly higher than that of the tung oilseed cake in the Comparative Examples. It also shows that the ultrasonic time, ultrasonic temperature, ethanol concentration, and solid-liquid ratio all have obvious effects on the extraction of polyphenols from the tung oilseed cake.

[0080] In summary, it can be seen that the use of the optimized process operation and parameter conditions described in the present invention to extract polyphenols from Alpinia oxyphylla cake can effectively solve the problem of poor effect in the Alpinia oxyphylla cake polyphenol extraction process in the prior art and significantly improve the extraction rate of polyphenols.

[0081] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for extracting polyphenols from Castanopsis schrenkiana cake, characterized in that: The steps include: (1) crushing and drying the tung oil tree cake obtained after the pretreatment to obtain tung oil tree cake powder; (2) mixing the Alpinia schrenkiana cake powder with 30-50% by volume ethanol, ultrasonically treating the mixture, and centrifuging the mixture to obtain an Alpinia schrenkiana cake powder polyphenol solution; (3) The polyphenol solution of the Castanopsis schrenkiana cake powder is rotary evaporated and concentrated to obtain the polyphenol solution.

2. The extraction method according to claim 1, characterized in that The crushed product in step (1) is passed through a sieve having a mesh size of 10-80 meshes.

3. The extraction method according to claim 1, characterized in that In step (2), the solid-liquid ratio of the mixture of the Castanopsis schrenkiana cake powder and ethanol is 1 g: (15-30) mL.

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

5. The extraction method according to claim 1, characterized in that The centrifugal speed in step (2) is 3000-4000 rpm, and the centrifugal time is 15-30 min.

6. The extraction method according to claim 1, characterized in that The step (2) is concentrated to 20-30% of the volume of the polyphenol solution of Castanopsis schrenkiana cake powder.

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