Method for jointly extracting essential oil, pectin and flavone from nymphaea candida presl

Abstract

The invention relates to a method for jointly extracting essential oil, pectin and flavone from nymphaea candida presl, and relates to the technical field of separation and extraction.The method comprises the following steps that nymphaea candida presl is subjected to steam distillation, and essential oil and distillation residues are obtained; the distillation residues are fermented and then filtered, and fermentation liquor is obtained; adding clear water into the fermentation liquor for cleaning, and performing rough filtration to obtain filtrate; carrying out pressurized extrusion filtration on the filtrate to obtain a pectin solution and filter residues; combining the pectin solution and an extracting solution prepared from the filter residues, concentrating and filtering, and then adding alcohol for precipitating to prepare pectin; and extracting the filter residues to obtain the flavone. The invention provides a method for jointly extracting essential oil, pectin and flavone from nymphaea candida presl for the first time, and the method has the characteristics of simple process, high extraction efficiency and the like.

Description

Technical Field

[0001] The invention relates to the technical field of separation and extraction, and in particular to a method for jointly extracting essential oil, pectin and flavonoids from water lilies. Background Art

[0002] Water lily is an aquatic herbaceous plant of the genus Nymphaeaceae, with a short, oblique or upright rhizome, and leaves that float on the water surface. They are round or oval, with three curved notches at the base, green on the upper side, dark purple-red on the lower side, and hairless on both sides. The leaf veins are fan-shaped, and the petiole is slender. The flower is solitary at the top of the long pedicel, floating on the water surface, and the vase is slightly square. The flowering period is from July to August. Water lily has the effects of clearing away heat and relieving summer heat, relieving alcohol, moistening the intestines and promoting bowel movements, and beautifying the skin, and has a wide range of uses.

[0003] At present, there are many reports on the extraction methods of the effective ingredients of water lily, such as CN106038713A reported a total flavonoid extract of water lily and its preparation method and application, CN114469814A reported a water lily extract and its preparation method and application, etc., but there are no reports in the prior art on the method of jointly extracting essential oil, pectin and flavonoids from water lily. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies.

[0005] The present invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies, the method comprising the following steps:

[0006] The water lily is subjected to steam distillation to obtain essential oil and distillation residue;

[0007] fermenting the distillation residue, and then filtering to obtain a fermentation liquid;

[0008] adding clean water to the fermentation liquid for washing and coarse filtering to obtain a filtrate;

[0009] The filtrate is subjected to pressure squeezing to obtain pectin liquid and filter residue;

[0010] The pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation to obtain pectin;

[0011] The filter residue is extracted to obtain flavonoids.

[0012] Furthermore, the working parameters of the steam distillation include: the steam distillation time is 2 hours.

[0013] Furthermore, the step of fermenting the distillation residue and then filtering to obtain the fermentation liquid comprises the following process:

[0014] Prepare sterile water with the same weight as the water lily raw material, dissolve 0.5-0.7 wt% of koji in the sterile water, and stir evenly to obtain koji liquid;

[0015] The koji liquid is poured into the distillation residue, statically fermented for 40 to 55 hours, and then filtered to obtain a fermentation liquid.

[0016] Furthermore, the added weight of the distiller's yeast is 0.6wt% of the weight of the water lily raw material; and the static fermentation time is 72 hours.

[0017] Furthermore, clean water is added to the fermentation liquid for washing and coarse filtration to obtain the filtrate, which includes the following process: adding clean water 2 to 3 times the weight of the water lily raw material to the fermentation liquid, soaking it for half an hour, changing the water twice, draining off the water, and obtaining the filtrate.

[0018] Furthermore, the working parameters of the pressurized filtration include: a pressure of 1.5 MPa.

[0019] Furthermore, the pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation. The step of preparing pectin includes the following process:

[0020] Add 2 to 3 times the weight of water to the filter residue, add sulfurous acid to adjust the pH value to 1.8 to 2.0, heat to 75° C., maintain for 45 to 60 minutes, and filter out the extract;

[0021] The obtained extract and the pectin solution are filtered with a 300-mesh filter bag respectively and combined, and then sent to a vacuum concentrator for concentration until the total solid weight content reaches 7wt% to 9wt%; 95% edible alcohol is slowly and gradually added in portions under stirring until no precipitation is generated; after standing, the alcohol is poured out, the filter is pressed, and the gelled pectin is taken out, and then 95% edible alcohol in an amount twice the weight of the pectin is used, stirred for 10 minutes to further wash the pectin, the filter is pressed, the pectin is taken out, and the gelled pectin is sent to a vacuum drying device for drying at 65 to 75°C to obtain the pectin.

[0022] Furthermore, the filter residue is extracted to obtain flavonoids, which comprises the following steps: adding the filter residue to the alcohol obtained after preparing pectin, heating to 65-85°C, maintaining for 30-40 minutes, and filtering out the alcohol extract; recovering the alcohol extract under reduced pressure and filtering the extract material through a filter press; standing until there is no alcohol taste, filtering with suction, and washing with sterile water to obtain a crude flavonoid; adding petroleum ether twice the weight of the crude flavonoid, soaking for half an hour, filtering, and continuing to wash with petroleum ether for several times, condensing and decompressing the petroleum ether to obtain flavonoids.

[0023] The above technical solution provided by the embodiment of the present invention has at least the following advantages compared with the prior art:

[0024] The invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies. The invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies for the first time, and has the characteristics of simple process, high extraction efficiency and the like. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0027] Figure 1 The present invention provides a schematic flow chart of a method for jointly extracting essential oil, pectin and flavonoids from water lilies. DETAILED DESCRIPTION

[0028] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. 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.

[0029] 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.

[0030] The present invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lily. Figure 1 As shown, the method comprises the following steps:

[0031] The water lily is subjected to steam distillation to obtain essential oil and distillation residue;

[0032] fermenting the distillation residue, and then filtering to obtain a fermentation liquid;

[0033] adding clean water to the fermentation liquid for washing and coarse filtering to obtain a filtrate;

[0034] The filtrate is subjected to pressure squeezing to obtain pectin liquid and filter residue;

[0035] The pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation to obtain pectin;

[0036] The filter residue is extracted to obtain flavonoids.

[0037] The invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies. The invention provides a method for jointly extracting essential oil, pectin and flavonoids from water lilies for the first time, and has the characteristics of simple process, high extraction efficiency and the like.

[0038] In some specific embodiments, the working parameters of the steam distillation include: the steam distillation time is 2 hours.

[0039] In some specific embodiments, the step of fermenting the distillation residue and then filtering to obtain the fermentation broth comprises the following process:

[0040] Prepare sterile water with the same weight as the water lily raw material, dissolve 0.5-0.7 wt% of koji in the sterile water, and stir evenly to obtain koji liquid;

[0041] The koji liquid is poured into the distillation residue, statically fermented for 40 to 55 hours, and then filtered to obtain a fermentation liquid.

[0042] In some specific embodiments, the weight of the added koji is 0.6wt% of the weight of the water lily raw material; and the static fermentation time is 72 hours.

[0043] In some specific embodiments, clean water is added to the fermentation liquid for washing and coarse filtration, and the step of obtaining the filtrate includes the following process: adding clean water accounting for 2 to 3 times the weight of the water lily raw material to the fermentation liquid, soaking it for half an hour, changing the water twice, draining off the water, and obtaining the filtrate.

[0044] In some specific embodiments, the working parameters of the pressurized filtration include: a pressure of 1.5 MPa.

[0045] In some specific embodiments, the pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation. The step of preparing pectin includes the following process:

[0046] Add 2 to 3 times the weight of water to the filter residue, add sulfurous acid to adjust the pH value to 1.8 to 2.0, heat to 75° C., maintain for 45 to 60 minutes, and filter out the extract;

[0047] The obtained extract and the pectin solution are filtered with a 300-mesh filter bag respectively and combined, and then sent to a vacuum concentrator for concentration until the total solid weight content reaches 7wt% to 9wt%; 95% edible alcohol is slowly and gradually added in portions under stirring until no precipitation is generated; after standing, the alcohol is poured out, the filter is pressed, and the gelled pectin is taken out, and then 95% edible alcohol in an amount twice the weight of the pectin is used, stirred for 10 minutes to further wash the pectin, the filter is pressed, the pectin is taken out, and the gelled pectin is sent to a vacuum drying device for drying at 65 to 75°C to obtain the pectin.

[0048] In some specific embodiments, the step of extracting the filter residue to obtain flavonoids includes the following process: adding the filter residue to the alcohol obtained after preparing pectin, heating to 65-85°C, maintaining for 30-40 minutes, and filtering out the alcohol extract; reducing pressure to recover the alcohol extract and filtering the extract material through a filter press; standing until there is no alcohol taste, filtering, and washing with sterile water to obtain a crude flavonoid; adding petroleum ether twice the weight of the crude flavonoid, soaking for half an hour, filtering, and continuing to wash with petroleum ether several times, condensing and reducing pressure to drain the petroleum ether to obtain flavonoids.

[0049] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples that do not specify specific conditions are usually measured according to national standards. If there is no corresponding national standard, then the conditions recommended by the manufacturer are followed.

[0050] Example 1

[0051] This example provides a method for jointly extracting essential oil, pectin and flavonoids from water lily, comprising the following steps:

[0052] 1. Distillation: Use steam distillation to extract essential oil from fresh materials; or steam for 5-10 minutes to inactivate pectinase and avoid pectin hydrolysis and reduced gelling degree;

[0053] 2. Fermentation: prepare sterile water of the same weight as the raw materials, dissolve 0.6% of the raw materials weight of koji in the water and stir evenly, pour the koji liquid into the raw materials that have been naturally cooled to the summer room temperature (25-32°C), cover, and ferment statically for 72 hours;

[0054] 3. Filter out the fermentation liquid, add clean water twice the weight of the raw material to the solid matter, soak for half an hour, change the water twice, and drain the water to remove the water-soluble substances contained in the raw materials, such as glycosides, sugars, acids, salts and bitterness, so as not to affect the quality of pectin;

[0055] 4. Squeeze and filter: Put the above raw materials into a gauze bag, place it in a pressurized filter, slowly pressurize it, and filter out the pectin liquid;

[0056] 5. Add 3 times the weight of water to the residue, add sulfurous acid to adjust the pH to 1.8-2.0; heat to 75°C, keep for 50 minutes, and filter out the extract;

[0057] 6. Concentration and storage of pectin liquid: Filter the extract obtained in step 5 with a 300-mesh filter bag, then send the pectin liquid into a vacuum concentration pot, maintain the vacuum degree above 667 mmHg, and the boiling point at about 50°C, and concentrate until the total solids reach 7-9%. Then filter the pectin obtained in step 4 with a 300-mesh filter bag and combine it with the extract;

[0058] 7. Heat the pectin solution to 70℃, put it into a glass bottle, cover and seal it, then place it in 70℃ hot water for heating and sterilization for 30 minutes. After cooling, send it to the warehouse, or put the pectin solution into a wooden barrel, add 0.2% sodium bisulfite, stir it evenly, and seal it for storage;

[0059] 8. Production of pectin powder: Slowly and gradually add 95% edible alcohol to the pectin solution obtained in step 6 under stirring (no rapid agglomeration should occur during this process) until no precipitation is generated;

[0060] 9. After standing, pour out the alcohol, filter, take out the gelled pectin, then use 95% edible alcohol twice the weight of the pectin, stir for 10 minutes to further wash the pectin, filter, take out the pectin, send the gelled pectin to a vacuum drying device, dry at 70°C (or freeze-dry) until the moisture content is less than 8%, then grind the pectin powder, sieve through a 60-mesh sieve, test, package, and store;

[0061] 10. Flavonoid extraction: add the filter residue obtained in step 4 to the alcohol obtained in step 9, heat to 70°C, keep for 35 minutes, and filter out the alcohol extract;

[0062] 11. Recover the alcohol extract under reduced pressure at 70℃. Filter the extract through a filter press until there is no alcohol taste. Let it stand at 5-8℃ for 3.5 hours, filter it with suction, and wash the crude product with sterile water several times.

[0063] 12. Add twice the weight of crude product petroleum ether with a boiling point range of 60-90℃, soak for half an hour, filter, continue to wash with a small amount of petroleum ether several times, condense and reduce pressure to drain the petroleum ether;

[0064] 13. Further evaporate the petroleum ether until it is odorless, dry it under negative pressure for 5 hours, test, package and store it.

[0065] Various embodiments of the present invention may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present invention; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, the range description from 1 to 6 should be considered to have specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.

[0066] The foregoing is merely a specific embodiment of the present invention, which enables those skilled in the art to understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features claimed herein.

Claims

1. A method for jointly extracting essential oil, pectin and flavonoids from water lilies, characterized in that: The method comprises the following steps: The water lily is subjected to steam distillation to obtain essential oil and distillation residue; fermenting the distillation residue, and then filtering to obtain a fermentation liquid; adding clean water to the fermentation liquid for washing and coarse filtering to obtain a filtrate; The filtrate is subjected to pressure squeezing to obtain pectin liquid and filter residue; The pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation to obtain pectin; The filter residue is extracted to obtain flavonoids.

2. The method according to claim 1, characterized in that The working parameters of the steam distillation include: the steam distillation time is 2 hours.

3. The method according to claim 1, characterized in that The step of fermenting the distillation residue and then filtering to obtain the fermentation liquid comprises the following process: Prepare sterile water with the same weight as the water lily raw material, dissolve 0.5-0.7 wt% of koji in the sterile water and stir evenly to obtain koji liquid; The koji liquid is poured into the distillation residue, statically fermented for 40 to 55 hours, and then filtered to obtain a fermentation liquid.

4. The method according to claim 3, characterized in that The added weight of the distiller's yeast is 0.6wt% of the weight of the water lily raw material; and the static fermentation time is 72 hours.

5. The method according to claim 1, characterized in that The step of adding clean water to the fermentation liquid for washing and coarse filtering to obtain the filtrate comprises the following process: adding clean water accounting for 2 to 3 times the weight of the water lily raw material to the fermentation liquid, soaking for half an hour, changing the water twice, draining off the water, and obtaining the filtrate.

6. The method according to claim 1, characterized in that The working parameters of the pressurized filtration include: a pressure of 1.5 MPa.

7. The method according to claim 1, characterized in that The pectin solution and the extract obtained from the filter residue are combined, concentrated and filtered, and then alcohol is added for precipitation. The step of preparing pectin includes the following process: Add 2 to 3 times the weight of water to the filter residue, add sulfurous acid to adjust the pH value to 1.8 to 2.0, heat to 75° C., maintain for 45 to 60 minutes, and filter out the extract; The obtained extract and the pectin solution are filtered with a 300-mesh filter bag respectively and combined, and then sent to a vacuum concentrator for concentration until the total solid weight content reaches 7wt% to 9wt%; 95% edible alcohol is slowly and gradually added in portions under stirring until no precipitation is generated; after standing, the alcohol is poured out, the filter is pressed, and the gelled pectin is taken out, and then 95% edible alcohol in an amount twice the weight of the pectin is used, stirred for 10 minutes to further wash the pectin, the filter is pressed, the pectin is taken out, and the gelled pectin is sent to a vacuum drying device for drying at 65 to 75°C to obtain the pectin.

8. The method according to claim 7, characterized in that The step of extracting the filter residue to obtain flavonoids includes the following process: adding the filter residue to the alcohol obtained after preparing pectin, heating to 65-85°C, maintaining for 30-40 minutes, and filtering out the alcohol extract; recovering the alcohol extract under reduced pressure and filtering the extract material through a filter press; standing until there is no alcohol taste, filtering with suction, washing with sterile water to obtain a crude flavonoid; adding petroleum ether twice the weight of the crude flavonoid, soaking for half an hour, filtering, continuing to wash with petroleum ether for several times, condensing and decompressing the petroleum ether to obtain flavonoids.

Images