Efficient extraction method for effective components of edible fresh flowers

Abstract

The invention provides a method for efficiently extracting effective components of edible fresh flowers, and relates to the technical field of fresh flower component extraction. The efficient extraction method for the effective components of the edible fresh flowers specifically comprises the following steps: S1, raw material preparation, S2, solvent addition, S3, ultrasonic extraction, S4, Soxhlet extraction, S5, filtration and concentration, S6, purification and separation, and S7, detection and analysis. The extraction efficiency of the ultrasonic coupling technique is generally superior to that of the traditional extraction method, the extraction efficiency of the target active component can be remarkably improved, the extraction time is shortened, and the quality of the extract is ensured. The technology has the advantages that plant cell walls can be destroyed, quick release of active ingredients is promoted, the use of organic solvents is reduced, the purity of bioactive compounds is improved, and the processing time and the operation cost are saved.

Description

Technical Field

[0001] The invention relates to the technical field of flower component extraction, in particular to a method for efficiently extracting effective components of edible flowers. Background Art

[0002] Edible flowers refer to flowers that are safe to eat. These flowers not only have an attractive appearance, but also add unique flavor and nutritional value to food. In addition to their decorative and flavor-enhancing effects, edible flowers are often rich in a variety of nutrients and phytochemicals. By extracting the active ingredients of these flowers, their nutrients and flavors can be concentrated and made easier for people to ingest. The extraction process can separate the aroma and taste components of the plant, which can be used in condiments, beverages, food additives, etc. to enhance the taste of food. Many edible flowers contain beneficial phytochemicals, and extracting these ingredients can help study their potential health benefits and even develop them into health supplements. The extracted ingredients are stored in a concentrated form, which is convenient for use in cooking and food processing, and also helps to extend the shelf life of the product and reduce transportation costs. Through extraction technology, a variety of new products can be developed, such as flower essences, flower teas, pollen, and extracts as health supplements, thereby enriching the product variety on the market. In general, the extraction of active ingredients can not only create economic value, but also promote people's attention and practice of healthy diet and lifestyle.

[0003] In the current extraction process, the traditional method that relies on the natural contact between the solvent and the sample is generally used. The extraction efficiency of this method is limited by the diffusion rate, resulting in low efficiency. Traditional extraction technology not only requires a large amount of organic solvents, which increases costs, but also burdens the environment. In addition, traditional technology usually takes a long time to achieve the extraction of effective ingredients, which reduces production efficiency. Due to the lack of efficient separation technology, the extracts obtained by traditional methods may contain more impurities and are not of high purity. Traditional extraction methods usually involve multi-step operations, including long-term heating, stirring, filtering, etc., and the operation is complicated. In addition, the organic solvents used in traditional methods may pollute the environment, and solvent volatilization may occur during the extraction process. Due to the need for a large amount of solvent and a long extraction time, the cost of traditional extraction methods is relatively high. Finally, traditional extraction methods rely on the experience and skills of the operator, which leads to poor reproducibility of extraction results. Summary of the invention

[0004] 1. Technical issues to be resolved

[0005] In view of the shortcomings of the prior art, the present invention provides a method for efficiently extracting effective ingredients from edible flowers, which solves the problems that the prior art does not use modern physical or chemical technologies to improve extraction efficiency, lacks efficient and automated extraction equipment, resulting in cumbersome operation and low efficiency; insufficient consideration of environmental impact and cost control; and difficulty in accurately controlling extraction conditions, such as temperature, time, solvent ratio, etc., resulting in poor consistency in extraction results.

[0006] (II) Technical solution

[0007] To achieve the above objectives, the present invention is implemented by the following technical scheme: a method for efficiently extracting effective components from edible fresh flowers, specifically comprising the following steps:

[0008] S1. Raw material preparation

[0009] Dry and crush edible flowers into particles to increase the contact area between solvent and raw materials and improve extraction efficiency;

[0010] S2. Add solvent

[0011] Mix the crushed flowers with the organic solvent methanol in a ratio of 3:1;

[0012] S3. Ultrasonic extraction

[0013] The sample solution was placed in an ultrasonic extractor for ultrasonic-assisted extraction, with a specific solid-liquid ratio of 1:17, an ethanol volume fraction of 62%, and an ultrasonic extraction time of 42 minutes;

[0014] S4. Soxhlet Extraction

[0015] After ultrasonic extraction, the samples were transferred to a Soxhlet extractor for Soxhlet extraction;

[0016] S5. Filtration and concentration

[0017] The fixed waste was filtered out using a filter membrane to obtain a solution, and then the solution was concentrated to a certain volume using a rotary evaporator;

[0018] S6. Purification and Isolation

[0019] Purify and separate the extracted solution using chromatography as needed to obtain active ingredients with higher purity;

[0020] S7. Detection and analysis

[0021] The reproducibility and predictability of the extraction process were analyzed, and weighted scores and predicted weighted scores were obtained.

[0022] Preferably, the Soxhlet extraction specifically includes the following steps: directly weighing the sample and placing it in the filter paper sleeve of the Soxhlet extractor, infiltrating the sample, performing the extraction operation according to the above method, installing the Soxhlet extraction device, connecting the components in the order, interfaces, and inlets and outlets, and assembling the extractor as required, rotating the knob to lock and fix the connecting components, placing the filter paper tube containing the sample in the extraction cylinder of the Soxhlet extractor, plugging the top of the filter paper tube, and then rotating the knob to connect and fix the extraction cylinder with the receiving bottle, adding anhydrous ethanol to the extraction cylinder, the amount added is 1 / 3 to 1 / 2 of the volume of the extraction cylinder, and then rotating the knob to connect and fix the extraction cylinder with the extractor, turning on the vacuum pump to keep the solvent in the extraction cylinder vibrating at a reciprocating frequency of 60 to 80 times per minute, and observing whether the extract drips into the receiving bottle smoothly. If not, the temperature can be appropriately adjusted or the cotton core can be replaced.

[0023] Preferably, the chromatographic method specifically comprises the following steps:

[0024] a. subjecting the extracted edible flower solution to appropriate pretreatment, including filtration and centrifugation, to remove solid particles or other impurities in the sample;

[0025] b. Rapid and green microextraction of pyrrolizidine alkaloids from edible flower solutions using UHPLC-MS / MS;

[0026] c. Use a Sh im-pack VP-ODS column (2.0 mm × 150 mm, 5 μm) for analysis, use a mixture of methanol and 0.1% formic acid as the mobile phase, the flow rate is 0.2 mL / min, separation is performed by gradient elution, and the column temperature is set to 30°C;

[0027] d. Inject the pretreated sample into the chromatographic column with an injection volume of 5 μL, and analyze the target compound using negative ion multiple reaction monitoring (MRM) mode;

[0028] e. Isoquercetin was isolated and prepared from cotton flower extract using HSCCC, using ethyl acetate-water (1:1) as a two-phase solvent system, the upper phase was the stationary phase, the lower phase was the mobile phase, the main engine speed was 800r / min, the volume flow rate was 2.0mL / min, and the detection wavelength was 254nm;

[0029] f. The structure of the obtained compound was identified by spectroscopy, and the purity of the product was determined by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC).

[0030] (III) Beneficial effects

[0031] The present invention provides a method for efficiently extracting effective ingredients from edible flowers. It has the following beneficial effects: the extraction method combines ultrasound-assisted Soxhlet extraction with chromatography technology, and compared with the prior art, it has achieved significant improvements in extraction efficiency, solvent dosage, processing time, selectivity, precision, sample preservation, stability of active ingredients, structural identification and quality control. It can greatly improve the extraction efficiency of the target active ingredients, shorten the operation time, and ensure the quality of the extract. The core advantage of this technology lies in its ability to destroy plant cell walls, promote the rapid release of active ingredients, reduce the consumption of organic solvents, improve the purity of bioactive compounds, and save processing time and cost. Therefore, it can extract effective ingredients from edible flowers more efficiently, environmentally friendly and accurately. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0033] Example 1: Ultrasonic assisted extraction

[0034] Sample preparation: Edible fresh flowers roses were crushed into particles of appropriate size.

[0035] Solvent extraction: Weigh 25 g of crushed rose sample and add 200 mL of 80% by volume methanol.

[0036] Ultrasonic extraction: Ultrasonic extraction was performed at 50°C for 30 minutes.

[0037] Filtration and concentration: Filter and combine the filtrates, remove methanol by rotary evaporation at 50°C, and lyophilize to obtain the stock solution.

[0038] Chromatographic purification: Purification and separation were performed using UHPLC-MS / MS with acetonitrile and water as the mobile phase, a flow rate of 1 mL / min, a column temperature of 25 °C, and an injection volume of 10 μL.

[0039] Example 2: Soxhlet extraction

[0040] Sample preparation: Cut the rose sample into pieces and put it into the Soxhlet extractor.

[0041] Soxhlet extraction: Use 250 mL of a mixture of ether and n-hexane (v:v=1:9) as the extraction solution, circulate 4 times / h, and extract for 16 hours.

[0042] Concentration and volume adjustment: The extract was concentrated to less than 1 mL in a rotary evaporator, blown to near dryness with nitrogen, and then adjusted to 1 mL with acetonitrile.

[0043] Chromatographic analysis: gradient elution was used.

[0044] Example 3: Ultrasonic Soxhlet Extraction

[0045] Sample preparation: After the rose sample was crushed, it was first subjected to ultrasonic pretreatment and then Soxhlet extraction.

[0046] Ultrasonic pretreatment: add 25 mL of acetonitrile and sonicate for 30 minutes at an oscillation frequency of 80 kHz.

[0047] Soxhlet extraction: Use a mixture of ether and n-hexane for Soxhlet extraction, cycle 4 times / h, and extract for 16 hours.

[0048] Chromatographic purification: Purification and separation were performed using UHPLC-MS / MS, optimized according to the fluorescence detector wavelength programming settings.

[0049] The final result of the efficient extraction method of active ingredients from edible flowers

[0050] Through the above examples, it can be seen that the combination of ultrasound-assisted Soxhlet extraction and chromatography can effectively extract active ingredients from edible flowers. This method solves the problems of low extraction efficiency, high solvent consumption, long extraction time, low purity, complex operation, large environmental impact, high cost and poor repeatability in traditional extraction methods. Specifically: Improved extraction efficiency: Ultrasonic assistance can accelerate the penetration of solvents into plant cells and destroy cell walls to release active ingredients.

[0051] Reduced solvent consumption: Ultrasonic pretreatment reduces the amount of organic solvents used.

[0052] Shortened extraction time: Ultrasonic extraction only takes 30 minutes, while Soxhlet extraction takes 16 hours, which greatly shortens the extraction time.

[0053] Improved purity: Chromatographic technology can efficiently purify and separate the extract to obtain high-purity active ingredients.

[0054] Simplified operation: The automated control system simplifies the operation process.

[0055] Reduced environmental impact: reduced consumption and emissions of organic solvents.

[0056] Cost reduction: Improved extraction efficiency, reduced solvent usage, and lowered overall extraction costs.

[0057] Improved reproducibility: Automated equipment improves the consistency and reproducibility of the extraction process.

[0058] The method used in the embodiment of the present invention is as follows:

[0059] A method for efficiently extracting effective components from edible flowers, comprising the following steps:

[0060] S1. Raw material preparation

[0061] Dry and crush edible flowers into particles to increase the contact area between solvent and raw materials and improve extraction efficiency;

[0062] S2. Add solvent

[0063] Mix the crushed flowers with the organic solvent methanol in a ratio of 3:1;

[0064] S3. Ultrasonic extraction

[0065] The sample solution was placed in an ultrasonic extractor for ultrasonic-assisted extraction, with a specific solid-liquid ratio of 1:17, an ethanol volume fraction of 62%, and an ultrasonic extraction time of 42 minutes;

[0066] S4. Soxhlet Extraction

[0067] After ultrasonic extraction, the sample is transferred to a Soxhlet extractor for Soxhlet extraction. The Soxhlet extraction specifically includes the following steps: directly weighing the sample and placing it in the filter paper sleeve of the Soxhlet extractor, soaking the sample, performing the extraction operation according to the above method, installing the Soxhlet extraction device, connecting the components in the order, interfaces, and inlets and outlets, and assembling the extractor as required, rotating the knob to lock and fix the connecting components, placing the filter paper tube containing the sample in the extraction cylinder of the Soxhlet extractor, plugging the top of the filter paper tube, and then rotating the knob to connect and fix the extraction cylinder with the receiving bottle, adding anhydrous ethanol to the extraction cylinder, the added amount is 1 / 3 to 1 / 2 of the volume of the extraction cylinder, and then rotating the knob to connect and fix the extraction cylinder with the extractor, turning on the vacuum pump to keep the solvent in the extraction cylinder vibrating at a reciprocating frequency of 60 to 80 times per minute, and observing whether the extract drips into the receiving bottle smoothly. If not, the temperature can be appropriately adjusted or the cotton core can be replaced;

[0068] S5. Filtration and concentration

[0069] The fixed waste was filtered out using a filter membrane to obtain a solution, and then the solution was concentrated to a certain volume using a rotary evaporator;

[0070] S6. Purification and Isolation

[0071] The extracted solution is purified and separated by chromatography as required to obtain active ingredients with higher purity. The chromatography method specifically includes the following steps:

[0072] a. subjecting the extracted edible flower solution to appropriate pretreatment, including filtration and centrifugation, to remove solid particles or other impurities in the sample;

[0073] b. Rapid and green microextraction of pyrrolizidine alkaloids from edible flower solutions using UHPLC-MS / MS;

[0074] c. Use a Sh im-pack VP-ODS column (2.0 mm × 150 mm, 5 μm) for analysis, use a mixture of methanol and 0.1% formic acid as the mobile phase, the flow rate is 0.2 mL / min, separation is performed by gradient elution, and the column temperature is set to 30°C;

[0075] d. Inject the pretreated sample into the chromatographic column with an injection volume of 5 μL, and analyze the target compound using negative ion multiple reaction monitoring (MRM) mode;

[0076] e. Isoquercetin was isolated and prepared from cotton flower extract using HSCCC, using ethyl acetate-water (1:1) as a two-phase solvent system, the upper phase was the stationary phase, the lower phase was the mobile phase, the main engine speed was 800r / min, the volume flow rate was 2.0mL / min, and the detection wavelength was 254nm;

[0077] f. The obtained compound was structurally identified by spectroscopy, and the purity of the product was determined by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC);

[0078] S7. Detection and analysis

[0079] The reproducibility and predictability of the extraction process were analyzed, and weighted scores and predicted weighted scores were obtained.

[0080] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for efficiently extracting effective ingredients from edible fresh flowers, characterized in that: The specific steps include: S1. Raw material preparation Dry and crush edible flowers into particles to increase the contact area between solvent and raw materials and improve extraction efficiency; S2. Add solvent Mix the crushed flowers with the organic solvent methanol in a ratio of 3:1; S3. Ultrasonic extraction The sample solution was placed in an ultrasonic extractor for ultrasonic-assisted extraction, with a specific solid-liquid ratio of 1:17, an ethanol volume fraction of 62%, and an ultrasonic extraction time of 42 minutes; S4. Soxhlet Extraction After ultrasonic extraction, the samples were transferred to a Soxhlet extractor for Soxhlet extraction; S5. Filtration and concentration The fixed waste was filtered out using a filter membrane to obtain a solution, and then the solution was concentrated to a certain volume using a rotary evaporator; S6. Purification and Isolation Purify and separate the extracted solution using chromatography as needed to obtain active ingredients with higher purity; S7. Detection and analysis The reproducibility and predictability of the extraction process were analyzed, and weighted scores and predicted weighted scores were obtained.

2. The method for efficiently extracting effective components from edible fresh flowers according to claim 1, characterized in that: The Soxhlet extraction specifically includes the following steps: directly weighing a sample and placing it in a filter paper sleeve of a Soxhlet extractor, soaking the sample, performing an extraction operation according to the above method, installing a Soxhlet extraction device, correspondingly connecting the components according to the order, interfaces, and inlets and outlets, and assembling the extractor as required, rotating the knob to lock and fix the connecting components, placing the filter paper tube containing the sample in the extraction cylinder of the Soxhlet extractor, plugging the top of the filter paper tube, and then rotating the knob to connect and fix the extraction cylinder with a receiving bottle, adding anhydrous ethanol to the extraction cylinder, the added amount is 1 / 3 to 1 / 2 of the volume of the extraction cylinder, and then rotating the knob to connect and fix the extraction cylinder with the extractor, turning on the vacuum pump to keep the solvent in the extraction cylinder vibrating at a reciprocating frequency of 60 to 80 times per minute, and observing whether the extract drips into the receiving bottle smoothly. If not, the temperature can be appropriately adjusted or the cotton core can be replaced.

3. The method for efficiently extracting effective components from edible fresh flowers according to claim 1, characterized in that: The chromatographic method specifically comprises the following steps: a. subjecting the extracted edible flower solution to appropriate pretreatment, including filtration and centrifugation, to remove solid particles or other impurities in the sample; b. Rapid and green microextraction of pyrrolizidine alkaloids from edible flower solutions using UHPLC-MS / MS; c. The analysis was performed using a Shim-packVP-ODS column (2.0 mm × 150 mm, 5 μm), using a mixture of methanol and 0.1% formic acid as the mobile phase, with a flow rate of 0.2 mL / min, and separation was performed by gradient elution. The column temperature was set at 30°C. d. Inject the pretreated sample into the chromatographic column with an injection volume of 5 μL, and analyze the target compound using negative ion multiple reaction monitoring (MRM) mode; e. Isoquercetin was isolated and prepared from cotton flower extract using HSCCC, using ethyl acetate-water (1:1) as a two-phase solvent system, the upper phase was the stationary phase, the lower phase was the mobile phase, the main engine speed was 800r / min, the volume flow rate was 2.0mL / min, and the detection wavelength was 254nm; f. The structure of the obtained compound was identified by spectroscopy, and the purity of the product was determined by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC).