Preparation method of passion fruit peel total saponins
Total saponins were extracted from passion fruit peel using ultrasound-assisted extraction and D-101 macroporous resin chromatography column technology, which solved the problem of waste of fruit peel resources and provided efficient resource utilization and environmental protection effects.
Patent Information
- Application Number
- CN202411345114.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-25
- Publication Date
- 2025-12-16
AI Technical Summary
Passion fruit processing results in significant waste of peel resources and failure to effectively utilize its bioactive compounds, leading to environmental pollution.
Total saponins were extracted from passion fruit peel using ultrasonic-assisted extraction combined with D-101 macroporous resin chromatography column technology. After concentration and drying, passion fruit peel extract powder with a total saponin content of more than 8% was prepared.
This method enables efficient extraction of total saponins from passion fruit peel, improving resource utilization, reducing environmental pollution, and providing a source of raw materials for functional food ingredients.
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of food technology, in particular to a preparation method of total saponins of passion fruit peel. BACKGROUND
[0002] Passion fruit, scientific name Passiflora edulis, is originally from Brazil. Its fruit tastes sour and sweet, and has a mixed flavor of various fruits, so it is named passion fruit. Passion fruit peel accounts for 50-55% of the mass of the fruit, and has great utilization potential, mainly because it contains bioactive compounds and nutrients, such as volatile oil, flavonoids, lipids and triterpenoids. The phytochemical properties in these residues can be used as functional food ingredients or for the manufacture of medicines, and are highly valued in the fields of food, medicine, cosmetics, etc. The behavior of taking juice and pulp and discarding the peel during the processing of passion fruit will cause great waste of resources and environmental pollution. SUMMARY
[0003] The present application relates to the field of food technology, in particular to a preparation method of total saponins of passion fruit peel.
[0004] The preparation method of total saponins of passion fruit peel is characterized by using passion fruit peel as raw material, and preparing passion fruit peel extract powder with total saponin content greater than 8% through the steps of pretreatment of column loading liquid, chromatography column extraction, concentration, drying, etc.
[0005] The preparation method of total saponins of passion fruit peel comprises the following steps: (1) Chromatography column extraction: After the dried passion fruit peel is crushed and passed through a 20-mesh sieve, ultrasonic-assisted extraction is carried out at room temperature according to a solid-liquid ratio (g:mL) of 1:15, with an ultrasonic power of 250 W and an ultrasonic time of 10 min, to obtain a mixture of extract and drug powder. The mixture of extract and drug powder is tied with gauze into several medicine bags, which are then transferred to a glass chromatography column. D-101 macroporous resin that has been treated is added to the glass chromatography column, with a small amount of water added to keep the medicine bags immersed in water. The column is collected at a flow rate of 0.4 mL / min according to a solid-liquid ratio (g:mL) of 1:15 as a collection unit, and a total of 3 collections are made. The collected liquids are combined to obtain passion fruit peel total saponin extract.
[0006] (2) Concentration and drying: The passion fruit peel total saponin extract is transferred to a rotary evaporator for vacuum concentration at a temperature not higher than 60℃, to obtain passion fruit peel total saponin extract, which is then placed in a vacuum drying oven for drying at a temperature not higher than 60℃, to obtain passion fruit peel extract powder. The total saponin content of the passion fruit peel extract powder is determined by vanillin-glacial acetic acid colorimetry, and the total saponin content is more than 8%.
[0007] In a preferred embodiment of the present application, the soaking solvent used in the soaking extraction step is water, and cellulase is added during the extraction, the extraction method is ultrasonic extraction, the extraction solvent is water, and the ultrasonic extraction conditions are an ultrasonic power of 250 W and an ultrasonic time of 10 minutes; in the purification step, D-101 macroporous resin dynamic adsorption and elution are used, the eluent used is 60% ethanol aqueous solution, the drying method is vacuum drying, and the total saponin content of the obtained passion fruit peel extract powder is greater than 8%.
[0008] The present application is further illustrated below with examples, but the scope of protection claimed by the present application is not limited to the following embodiments.
[0009] Example 1: A preparation method of passion fruit peel total saponins, comprising the following steps: (1) Chromatographic column extraction: dry passion fruit peel is crushed and passed through a 20-mesh sieve, 20 g of passion fruit peel powder is added according to a solid-liquid ratio (g:mL) of 1:15, 300 mL of water is added, and the mixture is mixed uniformly, then ultrasonic-assisted extraction is performed at room temperature, the ultrasonic power is 250 W, and the ultrasonic time is 10 min, thereby obtaining a mixture of the extract and the drug powder. The mixture of the extract and the drug powder is tied into a medicine bag with gauze, and then transferred to a glass chromatographic column, D-101 macroporous resin treated in advance is added to the glass chromatographic column, and the resin is attached with defatted cotton for buffering at the upper end, a small amount of water is added, the medicine bag is kept immersed in water, and collection is performed at a flow rate of 0.4 mL / min according to a solid-liquid ratio (g:mL) of 1:15 as a collection unit, a total of 560 mL of water extract is collected, then 60% ethanol aqueous solution as the total saponin extraction solvent is continuously added to the chromatographic column, and 560 mL of passion fruit peel total saponin extract is continuously collected.
[0010] (2) Concentration and drying: the passion fruit peel total saponin extract is transferred to a rotary evaporator for vacuum concentration, the concentration temperature is 55°C, passion fruit peel total saponin extract is obtained, which is placed in a vacuum drying oven for drying at 55°C, thereby obtaining passion fruit peel extract powder, the total saponin content of which is determined by vanillin-glacial acetic acid colorimetry, and the total saponin content is 8.57%.
[0011] Example 2: A preparation method of passion fruit peel total saponins, comprising the following steps: (1) Chromatographic column extraction: After crushing the dried passion fruit peel and passing it through a 20-mesh sieve, add 20g of passion fruit peel powder and 300mL of water at a solid-liquid ratio (g:mL) of 1:15. After mixing evenly, perform ultrasonic extraction at room temperature with an ultrasonic power of 250W and an ultrasonic time of 10min to obtain a mixture of extract and powder. Tie the mixture of extract and powder into several medicine bags with gauze and transfer them to a glass chromatography column. Add pre-treated D-101 macroporous resin to the glass chromatography column and attach defatted cotton for buffering at the top of the resin. Add a small amount of water to keep the medicine bags submerged. Collect at a flow rate of 0.4mL / min, with a solid-liquid ratio (g:mL) of 1:15 as one collection unit. Collect a total of 640mL of water extract. Then add 60% ethanol aqueous solution, the extraction solvent for total saponins, to the chromatography column and continue to collect 640mL of passion fruit peel total saponin extract.
[0012] (2) Concentration and drying: The total saponin extract of passion fruit peel was transferred to a rotary evaporator for vacuum concentration at a temperature of 50°C to obtain a total saponin extract of passion fruit peel. The extract was then placed in a vacuum drying oven and dried at 50°C to obtain passion fruit peel extract powder. The total saponin content was determined by the vanillin-glacial acetic acid colorimetric method, and the total saponin content was 8.83%.
[0013] Single-factor experiments were conducted to determine the optimal extraction solvent for total saponins from passion fruit peel, using the extraction rate of total saponins as the evaluation index. The absorbance of total saponins in the supernatant was used as the evaluation index to investigate the effects of ultrasonic power and ultrasonic time on the extraction efficiency. The extraction yield was used as the evaluation index to determine the required amount of extraction solvent to collect from passion fruit peel. To determine the extraction solvent amount for total saponins from passion fruit peel, a certain amount of anhydrous ethanol was prepared into extraction solvents with volume ratios of 10:0 (100% ethanol), 8:2 (80% ethanol), 6:4 (60% ethanol), 4:6 (40% ethanol), 2:8 (20% ethanol), and 0:10 (purified water). Weigh 1g of passion fruit peel powder into 6 portions, and place each portion into a 50mL Erlenmeyer flask. Add 20mL of extraction solvent of the corresponding volume ratio to each flask, shake on a shaker at room temperature for 1 hour, centrifuge at low temperature for 10 minutes, take an appropriate amount of supernatant, and measure its absorbance according to the method for determining total saponin content. Calculate the concentration of total saponins in the extract using the regression equation y = 45.491x - 0.0014, and calculate its extraction rate. The experimental results show that the extraction rates of total saponins are 16.82mg / g, 22.64mg / g, 23.59mg / g, 23.94mg / g, 22.99mg / g, and 13.93mg / g, respectively. The extraction rate of total saponins is highest when the extraction solvent is 60% ethanol aqueous solution. Therefore, the extraction solvent for total saponins from passion fruit peel is determined to be 60% ethanol aqueous solution.
[0014] To determine the absorbance volume (MV) of passion fruit peel, accurately weigh 1.0 g of passion fruit peel powder into 6 portions, add 20 mL of water to each portion, and shake on a shaker at room temperature for 0.5 h, 1 h, 2 h, 3 h, 4 h, and 5 h respectively. After the time is up, remove the portions, centrifuge at low temperature for 10 min, and obtain the supernatant. Measure the volume of the supernatant. Subtract the volume of the supernatant from the volume of solvent added, and calculate the water absorption (mL) of 1 g of passion fruit peel powder. This is the minimum water absorption volume. Continue adding water to the passion fruit peel powder after it has reached immersion equilibrium until the water just covers the powder. The minimum water absorption volume plus the added water is the minimum amount of solvent submerged. The experimental results show that the minimum water absorption volume of passion fruit peel powder is 7 mL, and the minimum amount of solvent submerged is 15 mL. Therefore, 1MV = 15 mL - 7 mL = 8 mL.
[0015] Determination of the ultrasonic-assisted extraction power of total saponins from passion fruit peel: 2g of passion fruit peel powder was weighed and divided into 5 portions. 30mL of water was added to each portion, and ultrasonic extraction was performed at room temperature with ultrasonic powers of 150W, 200W, 150W, 300W, and 350W, respectively. The extraction time was set to 10min, and extraction was performed once. After ultrasonic extraction, the mixture was removed and centrifuged at 6000r / min for 10min at low temperature to obtain 5 portions of supernatant. An appropriate amount of the supernatant was taken, and the absorbance of the centrifuged liquid was measured according to the method for determining the content of total saponins. The experimental results showed that the absorbance of total saponins was 0.533, 0.538, 0.557, 0.543, and 0.502, respectively. The absorbance of total saponins reached its peak at 250W. Therefore, the optimal ultrasonic-assisted extraction power was determined to be 250W.
[0016] Determination of the Ultrasonic-Assisted Extraction Time for Total Saponins from Passion Fruit Peel: Five portions of 2g passion fruit peel powder were extracted, each with 30mL of water. Ultrasonic extraction was performed at room temperature with a power of 250W for 5min, 10min, 15min, 25min, and 35min respectively, with each extraction performed only once. After ultrasonication, the mixture was centrifuged at low temperature for 10min. Five centrifuged liquids were obtained. An appropriate amount of the supernatant was taken, and the absorbance of the centrifuged liquid was measured according to the method for determining the total saponin content. The experimental results showed that the absorbances of total saponins were 0.477, 0.518, 0.489, 0.370, and 0.353, respectively. The optimal ultrasonic-assisted extraction time for passion fruit peel powder was determined to be 10min.
[0017] To determine the volume of the aqueous extract to be collected from passion fruit peel, 10g of passion fruit peel powder was weighed and placed in a three-necked flask. 150mL of water was added, and the mixture was stirred evenly with a glass rod. Ultrasonic extraction was performed under the conditions of 250W ultrasonic power and 10min extraction time. The extracted mixture was then wrapped in gauze to form several small packets, along with the extract, and placed in a well-sealed glass chromatography column lined with absorbent cotton. After the total saponins in the packets were fully dissolved, extraction was performed at a flow rate of 10mL / 15min. Aqueous extracts were collected sequentially at volumes of 1.5MV, 1.0MV, 1.0MV, and 0.5MV, for a total of four aliquots, with a total volume of 4MV. The remaining residue was extracted again with 1.5 mV of water using ultrasonic-assisted extraction under the same conditions as the ultrasonic extraction experiment described above. After filtration, another residue extract was obtained, resulting in a total of 5 aqueous extracts. A suitable amount of each aqueous extract was taken, and the absorbance of the centrifuged liquid was measured according to the method for determining the total saponin content. The concentration of total saponins in the extract was calculated using the regression equation y = 45.491x - 0.0014, and the mass of total saponins in each aqueous extract was calculated. The total amount of total saponins in the 4 mV aqueous extract and the residue extract was considered as 100%. The calculated extraction yields of total saponins in the aqueous extracts were 70.69%, 14.17%, 7.62%, 1.89%, and 5.63%, respectively. The above experimental results show that the total saponin extraction rate of the first three aqueous extracts accounts for about 92% of the total. Therefore, the solvent volume of the first three aqueous extracts can extract the total saponins from the passion fruit peel powder relatively completely. Thus, the collected volume of the aqueous extract of the passion fruit peel powder is 3.5 MV or greater than 3.5 MV.
Claims
1. A method for preparing total saponins from passion fruit peel, characterized in that... Passion fruit peel extract powder with a total saponin content greater than 8% was prepared by pretreatment of the loading solution, extraction by chromatography, concentration and drying.
2. The method for preparing total saponins from passion fruit peel as described in claim 1, characterized in that... Follow these steps: 1) Chromatographic column extraction: After crushing the dried passion fruit peel and passing it through a 20-mesh sieve, ultrasonic-assisted extraction was performed at room temperature at a solid-liquid ratio (g:mL) of 1:
15. The ultrasonic power was 250W and the ultrasonic time was 10min. The mixture of extract and powder was obtained. The mixture of extract and powder was tied into several medicine bags with gauze and then transferred to a glass chromatography column. The glass chromatography column was filled with pre-treated D-101 macroporous resin and the top of the resin was attached with degreased cotton for buffering. A small amount of water was added to keep the medicine bags submerged. The water was collected at a flow rate of 0.4mL / min, with a solid-liquid ratio (g:mL) of 1:15 as one collection unit. A total of 3 aqueous extracts were collected. The collected aqueous extracts were combined and set aside. Then, 60% ethanol aqueous solution, the extraction solvent for total saponins, was added to the chromatography column to continue collecting the total saponin extract of passion fruit peel. 2) Concentration and drying: The total saponin extract of passion fruit peel was transferred to a rotary evaporator for vacuum concentration at a temperature not exceeding 60°C to obtain a total saponin extract of passion fruit peel. This extract was then placed in a vacuum drying oven and dried at a temperature not exceeding 60°C to obtain passion fruit peel extract powder. The total saponin content was determined by the vanillin-glacial acetic acid colorimetric method, and the total saponin content was above 8%.
3. The preparation method according to claim 2, characterized in that... During column chromatography extraction, macroporous resin and passion fruit peel powder were packed in the same column. Passion fruit peel powder was placed in several gauze bags during packing. Macroporous resin was placed in the lower layer of the column, and passion fruit peel powder bags were added to the upper layer. The column was then eluted with water and extracted with 60% ethanol aqueous solution. The 60% ethanol extract was concentrated under reduced pressure, and the thick paste was dried under vacuum. The total saponin content of the obtained passion fruit peel extract powder was greater than 8%.