Preparation method and application of tangerine peel and dark tea extract

Abstract

The present invention relates to the technical field of extracts, and in particular to a method for preparing a tangerine peel and black tea extract and its application. The present invention uses water to extract black tea and tangerine peel to obtain an extract and an extraction residue, and the extract is concentrated and dried to obtain a dry material; then the extraction residue is further leached with an ethanol aqueous solution, the leaching solution is filtered and concentrated, and a composite extractant is used for extraction to obtain an extract, and then the solvent is removed to obtain a concentrated material; then the dry material and the concentrated material are combined to obtain the tangerine peel and black tea extract of the present invention. The present invention uses safe black tea and tangerine peel, which are both medicinal and edible, as raw materials, and the obtained extract product is safe and has excellent hypoglycemic, hypolipidemic and anti-oxidation effects.

Description

Technical Field

[0001] The invention relates to the technical field of extracts, and in particular to a preparation method and application of a tangerine peel and dark tea extract. Background Art

[0002] Tangerine peel black tea has high nutritional and medicinal value, and mainly contains active ingredients such as flavonoids, polyphenols and polysaccharides. Tangerine peel has the effects of regulating qi and strengthening the spleen, drying dampness and resolving phlegm. Its main chemical components include flavonoids, limonin, alkaloids, volatile oils, etc. Volatile oil is one of the important active substances in tangerine peel. At present, more than 160 compounds have been isolated and identified in tangerine peel volatile oil. Tangerine peel volatile oil has antioxidant activity, promotes digestive juice secretion, exhausts gas and softens blood vessels. As a post-fermented tea, black tea has the effect of expelling phlegm and lowering qi. It is rich in new components of natural growth metabolic compounds and microbial fermentation metabolism, including catechin compounds, flavonoids, phenolic acids, polysaccharides, alkaloids, terpenoid compounds and other ingredients.

[0003] Glucose and lipid metabolism diseases are often manifested as chronic metabolic diseases such as obesity or overweight, non-alcoholic fatty liver disease, type 2 diabetes, etc., which have sugar and lipid metabolism disorders as key triggering factors. Their key pathological points include insulin resistance, inflammation, intestinal flora imbalance, and oxidative stress, which pose a serious threat to human health.

[0004] At present, the treatment of glucose and lipid metabolism diseases often requires long-term medication, or even lifelong medication to control blood sugar and blood lipid levels to reduce complications such as cardiovascular and cerebrovascular diseases. In this process, some side effects of drugs are also difficult to avoid, especially adverse reactions such as liver damage and rhabdomyolysis caused by lipid-lowering drugs such as statins and fibrates, as well as gastrointestinal disorders and lactic acidosis caused by hypoglycemic drugs, which will reduce patients' medication compliance and quality of life.

[0005] Therefore, it is a technical problem that needs to be solved at present to provide a tangerine peel dark tea extract that is both medicinal and edible and can be used for lowering blood sugar, lowering blood lipids and anti-oxidation, which can take into account both efficacy and safety. Summary of the invention

[0006] The present invention is based on solving the above technical problems, and thus proposes the technical solution of the present invention. The technical solution of the present invention includes a preparation method of tangerine peel and dark tea extract and its application.

[0007] In one aspect, the present invention provides a method for preparing a tangerine peel and dark tea extract, comprising the following steps:

[0008] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 3-5:1 to obtain a mixed powder;

[0009] Step S2: mixing the mixed powder with 10-25 times the mass of water to obtain a liquid, stirring at 50-65° C. for 10-20 hours to obtain a stirred material; then filtering to obtain a filter residue and a filtrate; concentrating the filtrate under reduced pressure, and drying to obtain a dry material 1;

[0010] Step S3: mixing the filter residue of step S2 with 12-30 times the mass of ethanol aqueous solution, stirring at 45-60° C. for 4-10 hours to obtain a mixed material, filtering the mixed material, and concentrating under reduced pressure to obtain a concentrate 1;

[0011] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 10-20 times the mass, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure to remove the organic phase solvent, thereby obtaining a concentrate 2;

[0012] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 3-6:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2-3:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2-5%;

[0013] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:0.5-2 to obtain the tangerine peel dark tea extract.

[0014] Furthermore, in step S1, the powder is sieved to obtain a powder with a particle size between 0.05-1 mm.

[0015] Furthermore, in step S2, the filtration is performed using a filter membrane with a pore size of 1-10 microns.

[0016] Furthermore, in step S2, the temperature of the reduced pressure concentration is 58-65°C.

[0017] Furthermore, in step S2, the mixture is concentrated under reduced pressure to 0.7-1.5 times the mass of the powder.

[0018] Furthermore, in step S2, the drying is freeze-drying.

[0019] Furthermore, in step S2, the freeze-drying temperature is -45°C to -25°C.

[0020] Furthermore, in step S2, the mixture is dried until the water content by mass is less than 6.7%.

[0021] Furthermore, in step S3, the mass concentration of the ethanol aqueous solution is 40-65%.

[0022] Furthermore, in step S3, the filtration is performed using a filter membrane with a pore size of 0.1-0.5 microns.

[0023] Furthermore, in step S3, the temperature of the reduced pressure concentration is 54-58°C.

[0024] Furthermore, in step S3, the pressure of reduced pressure concentration is 0.005-0.01 MPa.

[0025] Furthermore, in step S3, the mixture is concentrated under reduced pressure to 0.5-1.2 times the mass of the powder.

[0026] Furthermore, in step S4, the extraction temperature is 35-48° C., and the extraction time is 4-8 hours.

[0027] Furthermore, in step S4, the temperature of the reduced pressure concentration is 52-56° C. and the pressure is 0.012-0.02 MPa.

[0028] Furthermore, in step S4, when the organic phase solvent is no longer detected during the reduced pressure concentration, the concentration is stopped to obtain the concentrate 2.

[0029] On the other hand, the present invention also provides a tangerine peel dark tea extract prepared by the preparation method.

[0030] On the other hand, the present invention also provides a use of the tangerine peel and dark tea extract in preparing health products or medicines.

[0031] On the other hand, the present invention also provides a use of the tangerine peel and dark tea extract in preparing a lipid-lowering or antioxidant preparation.

[0032] Beneficial effects:

[0033] The present invention uses water to extract dark tea and tangerine peel to obtain an extract and an extraction residue, and the extract is concentrated and dried to obtain a dry material; then the extraction residue is further leached with an ethanol aqueous solution, the leaching solution is filtered and concentrated, and a composite extractant is used for extraction to obtain an extract, and then the solvent is removed to obtain a concentrated material; then the dry material and the concentrated material are combined to obtain the tangerine peel dark tea extract of the present invention. The tangerine peel dark tea extract has excellent hypoglycemic, hypolipidemic and anti-oxidation effects.

[0034] After the diabetic model was established, the blood sugar level of the experimental mice was reduced to 6.04 mmol / L after using the extract of the present invention for 4 weeks. The extract of the present invention has a significant effect on lowering blood sugar.

[0035] After the diabetic model was established, after using the extract of the present invention for 4 weeks, the concentrations of TG, TC and LDL-C in the blood of the experimental mice were reduced to 0.88±0.09mmol / L, 1.08±0.15mmol / L and 0.34±0.04mmol / L, respectively, and the concentration of HDL-C was as high as 1.41±0.19mmol / L; the extract of the present invention has an excellent lipid-lowering effect.

[0036] After the extract of the present invention is diluted to 5wt%, the DPPH free radical scavenging rate reaches 87.63%, and has excellent anti-oxidation and anti-aging effects.

[0037] The selection of the dosage ratio of dark tea and tangerine peel in the extraction system of the present invention has a greater influence on the effects of lowering blood sugar, lowering blood lipids and scavenging free radicals. When the mass ratio of dark tea to tangerine peel is in the range of 3-5:1, the overall effect of the extract is better.

[0038] The present invention adjusts the extraction process to make the extract more effective. The organic phase solvent in the extracting agent of the present invention uses a combination of ethyl acetate and cyclohexane, which can mutually promote the hypoglycemic and anti-oxidative effects of the extract. When the ratio of the two reaches 2-3:1, the extract has a better effect.

[0039] The present invention optimizes the dosage relationship between the dry material 1 and the concentrate 2, so that the effect of the extract is more significant.

[0040] The invention adopts safe black tea and tangerine peel which are both medicinal and edible as raw materials, and the obtained extract product is safe and has excellent blood sugar lowering, blood lipid lowering and antioxidant effects. DETAILED DESCRIPTION

[0041] The present invention will be described below in conjunction with specific embodiments, and various effects of the present invention will be more clearly presented. It should be understood by those skilled in the art that these specific embodiments are used to illustrate the present invention, rather than to limit the present invention.

[0042] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

[0043] Source of raw materials: Dark tea: The dark brick tea in Mucang dark tea comes from Hunan Anhua No. 1 Tea Factory Co., Ltd. of China Tea; Tangerine peel: Xinhui tangerine peel comes from Beijing Tong Ren Tang; Ethanol: CAS No. 64-17-5; Ethyl acetate: CAS No. 141-78-6; Cyclohexane: CAS No. 110-82-7.

[0044] 1. Preparation of Extracts

[0045] Extract 1: The preparation method is as follows:

[0046] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4.5:1 to obtain a mixed powder;

[0047] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0048] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0049] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0050] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0051] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0052] Extract 2: The preparation method is as follows:

[0053] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 3:1 to obtain a mixed powder;

[0054] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 50° C. for 17 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced pressure concentrated at a temperature of 63° C. and a pressure of 0.007 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.1% by mass to obtain a dry material 1;

[0055] Step S3: mixing the filter residue of step S2 with 25 times the mass of 40wt% ethanol aqueous solution, stirring at 50°C for 7 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 56°C and a pressure of 0.007MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0056] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 17 times the mass, and the mixture is extracted at a temperature of 38° C. for 6.5 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 53° C. and a pressure of 0.017 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0057] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 6:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 3.2%;

[0058] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.5 to obtain the tangerine peel dark tea extract.

[0059] Extract 3: The preparation method is as follows:

[0060] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 0.5:1 to obtain a mixed powder;

[0061] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0062] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0063] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0064] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0065] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0066] Extract 4: The preparation method is as follows:

[0067] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 1.5:1 to obtain a mixed powder;

[0068] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0069] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0070] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0071] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0072] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0073] Extract 5: The preparation method is as follows:

[0074] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 7:1 to obtain a mixed powder;

[0075] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0076] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0077] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0078] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0079] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0080] Extract 6: The preparation method is as follows:

[0081] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0082] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0083] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0084] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0085] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is ethyl acetate, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0086] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0087] Extract 7: The preparation method is as follows:

[0088] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0089] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0090] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0091] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0092] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is cyclohexane, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0093] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0094] Extract 8: The preparation method is as follows:

[0095] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0096] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0097] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0098] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0099] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 0.8:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0100] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0101] Extract 9: The preparation method is as follows:

[0102] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0103] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0104] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0105] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0106] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0107] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:1.2 to obtain the tangerine peel dark tea extract.

[0108] Extract 10: The preparation method is as follows:

[0109] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0110] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0111] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0112] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0113] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0114] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:0.1 to obtain the tangerine peel dark tea extract.

[0115] Extract 11: The preparation method is as follows:

[0116] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0117] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0118] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0119] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0120] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0121] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:0.25 to obtain the tangerine peel dark tea extract.

[0122] Extract 12: The preparation method is as follows:

[0123] Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder with a particle size of 0.05-1 mm, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 4:1 to obtain a mixed powder;

[0124] Step S2: mixing the mixed powder with 20 times the mass of water to obtain a feed liquid, stirring at 52° C. for 15 hours to obtain a stirred material; then filtering using a filter membrane with a pore size of 5 microns to obtain a filter residue and a filtrate; the filtrate is reduced in pressure and concentrated at a temperature of 62° C. and a pressure of 0.009 MPa to 1 times the mass of the mixed powder, and then freeze-dried at a temperature of -35° C. to a water content of about 5.2% to obtain a dry material 1;

[0125] Step S3: mixing the filter residue of step S2 with 25 times the mass of 55wt% ethanol aqueous solution, stirring at 55°C for 8 hours to obtain a mixed material, filtering the mixed material using a filter membrane with a pore size of 0.22 micron, and concentrating the filtrate under reduced pressure at a temperature of 55°C and a pressure of 0.0075MPa to 1 times the mass of the mixed powder, to obtain a concentrate 1;

[0126] Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 15 times the mass, and the mixture is extracted at a temperature of 38° C. for 6 hours, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure at a temperature of 52.5° C. and a pressure of 0.016 MPa to remove the organic phase solvent. When the organic phase solvent cannot be detected during the reduced pressure concentration, the concentration is stopped to obtain a concentrate 2;

[0127] The mass ratio of the organic phase to the inorganic phase in the composite extractant is 4.2:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2.5:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2.8%;

[0128] Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:4 to obtain the tangerine peel dark tea extract.

[0129] 2. Effect Test

[0130] 1. Test on the effect of extract on lowering blood sugar and blood lipid

[0131] SPE grade Kunming male mice weighing about 22±3g were taken and adaptively fed for 1 week. The mice were randomly divided into a blank control group and a model group; the blank control group was fed with conventional feed for 1 hour; the model group mice were fed with high-sugar and high-fat feed, wherein the high-sugar and high-fat feed composition was: 22wt% lard, 18wt% egg yolk powder, 12wt% sucrose, 2.5wt% cholesterol, 0.8wt% bile salt and the rest of conventional feed. After 30 days, fasting for 8h, the blank group mice were intraperitoneally injected 4 times with pH 4.5 citric acid buffer 40mg / kg per hour, and the model group mice were given STZ solution (prepared with pH 4.5 citric acid buffer) 40mg / kg intraperitoneally 4 times, once a day; continue to feed each group of mice with the same feed. One week after STZ injection, blood was collected from the tail vein of the mice in the model group to measure the blood sugar level. The blood sugar level above 14mmol / L indicated that the diabetic model mice in the model group were successfully modeled.

[0132] The mice in the above-mentioned successful model group were randomly divided into a model control group, an experimental group (divided into the above-mentioned extract groups 1-12), and a drug group, with 10 mice in each specific group having successful modeling. The above-mentioned blank control group and drug group were used as controls with the experimental group. The experimental group was given oral administration every hour, and the dosage of crude drug was 220 mg / kg / d; the model control group and the blank control group were given oral administration of normal saline, the amount was 220 mg / kg / d; the drug group was given oral administration of metformin, and the dosage of metformin was 180 mg / kg / d. Each group was given oral administration once a day for 4 consecutive weeks. One day before the end of the oral administration experiment, the rats fasted for 12 hours, and blood was taken to measure the fasting blood glucose value and TG, TC, LDL-C, and HDL-C values; the specific test comparison results are shown in Tables 1 and 2.

[0133] Table 1: Comparison of blood glucose levels in each group of mice

[0134]

[0135]

[0136] Table 2: Comparison of TG, TC, LDL-C, and HDL-C values ​​in each group of mice after 4 weeks of oral administration

[0137]

[0138]

[0139] 2. Antioxidant Effect Test of Extracts

[0140] The extracts 1-12 were diluted to a mass concentration of 5% using an ethanol aqueous solution with a mass concentration of 60% to obtain a test solution.

[0141] 4 mL of a concentration of 6.5 × 10 -5 mol / L DPPH aqueous solution was added to 4 mL of the above test solution, mixed evenly, and the absorbance value was measured at 518 nm, recorded as Ai; then it was placed at room temperature and protected from light for half an hour, and the absorbance value at 518 nm was measured, recorded as Aj. The concentration was then measured to be 6.5×10 -5 The absorbance value of the DPPH solution of 10 mol / L at 518 nm is recorded as Ac. The scavenging rate of the above-mentioned different extract solutions on DPPH free radicals is calculated by the formula of scavenging rate / %=[1-(Ai-Aj) / Ac]×100%. The results of the scavenging rate of the solutions of each extract on DPPH free radicals are shown in Table 3.

[0142] Table 3: DPPH free radical scavenging rate of each extract solution

[0143]

[0144]

[0145] According to the test results in Tables 1-3, the present invention extracts dark tea and tangerine peel with water to obtain an extract and an extract residue, concentrates the extract, and dries it to obtain a dry material; then the extract residue is further leached with an ethanol aqueous solution, the extract is filtered, concentrated, and extracted with a composite extractant to obtain an extract, which is then treated by removing the solvent to obtain a concentrated material; then the dry material and the concentrated material are combined to obtain the tangerine peel dark tea extract of the present invention. The tangerine peel dark tea extract has excellent hypoglycemic, hypolipidemic and anti-oxidative effects.

[0146] It can be seen from the test results in Table 1 that after the diabetic model was established, the blood sugar level of the mice decreased by 6.04 mmol / L after using the extract of the present invention for 4 weeks. The extract of the present invention has a significant effect on lowering blood sugar.

[0147] The test results in Table 2 show that after the diabetic model was established, after using the extract of the present invention for 4 weeks, the concentrations of TG, TC, and LDL-C in the blood of mice were as low as 0.88±0.09mmol / L, 1.08±0.15mmol / L, and 0.34±0.04mmol / L, respectively, and the concentration of HDL-C was as high as 1.41±0.19mmol / L; the extract of the present invention has an excellent lipid-lowering effect.

[0148] The test results in Table 3 show that after the extract of the present invention is diluted to 5wt%, the DPPH free radical scavenging rate reaches 87.63%, which has excellent antioxidant and anti-aging effects.

[0149] It can be seen from the test results of extract groups 1-5 in Tables 1-3 that the selection of the dosage ratio of black tea and tangerine peel in the extraction system of the present invention has a greater impact on the effects of lowering blood sugar, lowering blood lipids and scavenging free radicals. When the mass ratio of black tea to tangerine peel is in the range of 3-5:1, the overall effect of the extract is better.

[0150] It can be known from the test results of extracts 1, 6-9 in Table 1-3 that the present invention adjusts the extraction process to make the extract more effective. The organic phase solvent in the extractant of the present invention uses ethyl acetate and cyclohexane, which can mutually promote the hypoglycemic and anti-oxidative effects of the extract. When the ratio of the two reaches 2-3:1, the extract has a better effect.

[0151] It can be seen from the test results of extracts 1 and 10-12 in Tables 1-3 that the present invention optimizes the dosage relationship between the dry material 1 and the concentrate 2, making the effect of the extract more significant.

[0152] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A method for preparing tangerine peel and dark tea extract, characterized in that: The steps include: Step S1: crushing dark tea and tangerine peel respectively, sieving to obtain powder, and mixing the dark tea powder and tangerine peel powder in a mass ratio of 3-5:1 to obtain a mixed powder; Step S2: mixing the mixed powder with 10-25 times the mass of water to obtain a liquid, stirring at 50-65° C. for 10-20 hours to obtain a stirred material; then filtering to obtain a filter residue and a filtrate; concentrating the filtrate under reduced pressure, and drying to obtain a dry material 1; Step S3: mixing the filter residue of step S2 with 12-30 times the mass of ethanol aqueous solution, stirring at 45-60° C. for 4-10 hours to obtain a mixed material, filtering the mixed material, and concentrating under reduced pressure to obtain a concentrate 1; Step S4: the concentrate 1 is mixed with a composite extractant composed of an organic phase solvent and an inorganic phase in an amount of 10-20 times the mass, and then the inorganic phase is poured out, and the organic phase after extraction is concentrated under reduced pressure to remove the organic phase solvent, thereby obtaining a concentrate 2; The mass ratio of the organic phase to the inorganic phase in the composite extractant is 3-6:1; the organic phase is composed of ethyl acetate and cyclohexane in a mass ratio of 2-3:1, and the inorganic phase is a calcium chloride solution with a mass concentration of 2-5%; Step S5: combining the dried material 1 and the concentrate 2 in a mass ratio of 1:0.5-2 to obtain the tangerine peel dark tea extract; In step S3, the mass concentration of the ethanol aqueous solution is 40-65%; In step S4, the extraction temperature is 35-48° C. and the extraction time is 4-8 hours.

2. The preparation method according to claim 1, characterized in that In step S2, the temperature of reduced pressure concentration is 58-65°C, and the reduced pressure concentration is performed to 0.7-1.5 times the mass of the mixture powder.

3. The preparation method according to claim 1, characterized in that: In step S2, the drying is freeze-drying, and the drying is performed until the water content by mass is less than 6.7%.

4. The preparation method according to claim 1, characterized in that: In step S3, the temperature of reduced pressure concentration is 54-58° C., and the reduced pressure concentration is performed to 0.5-1.2 times the mass of the mixture powder.

5. The preparation method according to claim 1, characterized in that: In step S4, the temperature of reduced pressure concentration is 52-56° C. and the pressure is 0.012-0.02 MPa.

6. A tangerine peel and dark tea extract prepared according to the preparation method according to any one of claims 1 to 5.

7. Use of the tangerine peel and dark tea extract according to claim 6 in preparing health products or medicines.

8. Use of the tangerine peel and dark tea extract according to claim 6 in the preparation of lipid-lowering or antioxidant preparations.

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