CN115261142A - Saffron extraction process and device - Google Patents

Saffron extraction process and device Download PDF

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Publication number
CN115261142A
CN115261142A CN202211038798.XA CN202211038798A CN115261142A CN 115261142 A CN115261142 A CN 115261142A CN 202211038798 A CN202211038798 A CN 202211038798A CN 115261142 A CN115261142 A CN 115261142A
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saffron
tank
pipe
extraction
filtrate
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张春颖
许波
杨旭锦
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Tibet Tianhong Technology Co ltd
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Tibet Tianhong Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a saffron extraction process, which comprises the following steps: freezing stigma croci at low temperature below-20 deg.C, and crushing and grinding after all stigma croci is embrittled at low temperature; adding saffron crocus powder into an ethanol solution, carrying out low-temperature ultrasonic extraction, filtering to obtain a first filtrate, adding the filtered first filter residue into the ethanol solution, carrying out low-temperature ultrasonic extraction, filtering to obtain a second filtrate, adding the filtered second filter residue into the ethanol solution, carrying out low-temperature ultrasonic extraction, and filtering to obtain a third filtrate; mixing the first filtrate, the second filtrate and the third filtrate to obtain crude saffron extract, inactivating enzyme with high-pressure carbon dioxide, continuously extracting under reflux for 2 hr, and filtering to obtain saffron extract; vacuum concentrating the extractive solution, and vacuum drying to obtain stigma croci Sativi extract. The invention can effectively improve the extraction amount of the components such as crocin, total flavone and the like.

Description

Saffron extraction process and device
Technical Field
The invention relates to the field of Tibetan medicine extraction. More particularly, the present invention relates to a saffron extraction process and apparatus.
Background
Saffron, a perennial flower of crocus in iridaceae, is also a common perfume. Is a southwestern Asia protospecies which is artificially cultivated by Greek at first. It is mainly distributed in Europe, mediterranean region and Central Asia region, and introduced into China in Ming dynasty, and is listed as a herb in compendium of materia Medica, and planted in Zhejiang region. Is a rare Chinese medicinal material, has strong physiological activity, has effects of tranquilizing, eliminating phlegm, and relieving spasm, and can be used for treating gastropathy, regulating menstruation, measles, fever, jaundice, hepatosplenomegaly, etc.
At present, the extraction method of the effective components in the saffron is generally an alcohol extraction method under normal temperature and pressure, the raw materials are dried and crushed firstly, and the plant enzymes in the saffron are not inactivated, so that the plant enzymes can easily decompose part of the effective components in the saffron in the processes of crushing the raw materials and extracting alcohol, and the extraction amount of the effective components in the saffron is reduced.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and to provide at least the advantages described hereinafter.
Still another object of the present invention is to provide a process and apparatus for extracting saffron, which can effectively increase the content of effective components in the saffron extract.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a saffron extraction process comprising the steps of:
step one, freezing saffron at a low temperature below-20 ℃, crushing and grinding the saffron until the particle size is 80 meshes and the particle size is fine after all the saffron is embrittled at the low temperature;
step two, adding the saffron crocus powder prepared in the step one into an ethanol solution with the volume fraction of 60%, carrying out low-temperature ultrasonic extraction for 2-3 h at the temperature of 0-4 ℃, filtering to obtain a first filtrate, adding the filtered first filter residue into the ethanol solution with the volume fraction of 70%, carrying out low-temperature ultrasonic extraction for 1-1.5 h at the temperature of 0-4 ℃, filtering to obtain a second filtrate, adding the filtered second filter residue into the ethanol solution with the volume fraction of 75%, carrying out low-temperature ultrasonic extraction for 30-40 min at the temperature of 0-4 ℃, and filtering to obtain a third filtrate;
step three, combining the first filtrate, the second filtrate and the third filtrate prepared in the step two to obtain a saffron crude extraction liquid, inactivating enzyme by adopting high-pressure carbon dioxide, continuously performing low-pressure reflux extraction for 2 hours at 60 ℃ and under the condition of 15-20 kpa, and filtering to obtain a saffron crocus essence extracting solution;
and step four, carrying out reduced pressure concentration on the saffron crocus essence extracting solution prepared in the step three, adjusting the pH value to 7.0-7.5, and carrying out vacuum drying to obtain the saffron crocus extract.
Preferably, in the second step, the material-to-liquid ratio of the saffron powder to the ethanol solution with the volume fraction of 60% is 1.
Preferably, the ultrasonic power used for low-temperature ultrasonic extraction in the step two is 500W, and the circulating cooling water is adopted to maintain the ethanol solution at 0-4 ℃ in the low-temperature ultrasonic extraction process.
Preferably, the saffron crude extract in the third step is supercritical CO at 30MPa and 35 deg.C 2 And (3) inactivating the enzyme for 1 hour by using high-pressure carbon dioxide.
Preferably, said saffron extract is used to make granules, tablets or capsules.
The invention also provides a saffron extraction device, which is used for the low-pressure reflux extraction process in the third step in the saffron extraction process, and the saffron extraction device comprises:
the heating tank is provided with a water feeding pipe on the wall, a water discharging pipe is arranged at the bottom of the heating tank, a first valve is arranged at the orifice of the water discharging pipe, and an electric heating coil pipe is also arranged in the heating tank;
the material tank is arranged in the heating tank, the electric heating coil pipe surrounds the material tank, a charging pipe is arranged on the tank wall of the material tank, the charging pipe penetrates out of the tank wall of the heating tank, a second valve is arranged at the pipe orifice of the charging pipe, a steam pipe is arranged at the top of the material tank, and the steam pipe penetrates out of the top of the heating tank;
the condenser comprises a conical container, a plurality of condensing pipes, a condensing tank and a cooling water tank, wherein the top of the conical container is connected with a steam pipe penetrating out of the top of the heating tank, the bottom of the conical container is connected with the plurality of condensing pipes in parallel, the bottoms of the plurality of condensing pipes are connected with the top of the condensing tank, the bottom of the condensing tank is higher than the liquid level of materials in the material tank, the conical container, the plurality of condensing pipes and the condensing tank are all arranged in the cooling water tank, a water outlet is formed in the upper part of the wall of the cooling water tank, and a water inlet is formed in the lower part of the wall of the cooling water tank;
the bottom of the condensing tank is provided with a return pipe, the return pipe penetrates out of the wall of the cooling water tank and penetrates into the heating tank to be connected with the bottom of the material tank, a vacuum pump is further arranged outside the heating tank and connected with an exhaust pipe, the exhaust pipe penetrates into the heating tank to be communicated with the material tank, and a third valve is arranged on the exhaust pipe.
Preferably, an extracting solution discharging pipe is arranged at the bottom of the material tank, penetrates out of the bottom of the heating tank, and a fourth valve is arranged at the pipe orifice of the extracting solution discharging pipe.
Preferably, a three-way joint is arranged between the return pipe and the condensing tank, one end of the three-way joint is connected with the bottom of the condensing tank, the other end of the three-way joint is connected with the return pipe, the third end of the three-way joint is connected with a solvent discharge pipe, the solvent discharge pipe penetrates out of the bottom of the cooling water tank, and a fifth valve is arranged at the pipe orifice of the solvent discharge pipe.
Preferably, a sixth valve is provided on the return pipe.
The invention at least comprises the following beneficial effects: the invention well retains the active ingredients in the saffron crocus by low-temperature crushing, utilizes low-temperature alcohol extraction to avoid the decomposition of the active ingredients by enzyme in plants, then carries out enzyme inactivation, low-pressure reflux extraction and further purification, and avoids the oxidative decomposition failure of the active ingredients at high temperature due to low temperature of the low-pressure reflux extraction. Meanwhile, the saffron extraction device provided by the invention can be used for carrying out continuous reflux extraction under low pressure, and has high production efficiency and good purification effect.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
Fig. 1 is a schematic structural diagram of a saffron extraction device according to an embodiment of the present invention;
the device comprises a heating tank 1, a water adding pipe 2, a water discharging pipe 3, a first valve 4, an electric heating coil 5, a material tank 6, a feeding pipe 7, a second valve 8, a steam pipe 9, a conical container 10, a condenser pipe 11, a condenser pipe 12, a cooling water tank 13, a water outlet 14, a water inlet 15, a return pipe 16, a vacuum pump 17, an air pumping pipe 18, a third valve 19, an extracting solution discharge pipe 20, a fourth valve 21, a solvent discharge pipe 22, a fifth valve 23 and a sixth valve 24.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials, if not otherwise specified, are commercially available; in the description of the present invention, the terms "lateral", "longitudinal", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
< example 1>
A stigma croci Sativi extraction process comprises the following steps:
step one, freezing saffron at a low temperature below-20 ℃, crushing and grinding the saffron until the particle size is 80 meshes and the particle size is fine after all the saffron is embrittled at the low temperature;
step two, adding the saffron powder prepared in the step one into an ethanol solution with a volume fraction of 60%, wherein the material-liquid ratio of the saffron powder to the ethanol solution with a volume fraction of 60% is 1;
step three, combining the first filtrate, the second filtrate and the third filtrate prepared in the step two to obtain a saffron crude extraction liquid, and performing supercritical CO treatment on the saffron crude extraction liquid at the temperature of 35 ℃ under the pressure of 30MPa to obtain the saffron crude extraction liquid 2 Inactivating enzyme for 1h by high-pressure carbon dioxide, continuously extracting for 2h by low-pressure reflux at 60 ℃ under the condition of 15-20 kpa, and filtering to obtain saffron essence extract;
and step four, carrying out reduced pressure concentration on the saffron crocus essence extracting solution prepared in the step three, adjusting the pH value to 7.0, and carrying out vacuum drying to obtain the saffron crocus extract.
By adopting the method, 83.32g saffron extract can be obtained from 1kg saffron.
< example 2>
A stigma croci Sativi extraction process comprises the following steps:
step one, freezing saffron at low temperature, wherein the freezing temperature is below-20 ℃, crushing and grinding the saffron until the particle size is 80 meshes and fine after all saffron are embrittled at low temperature;
step two, adding the saffron powder prepared in the step one into an ethanol solution with a volume fraction of 60%, wherein the material-liquid ratio of the saffron powder to the ethanol solution with a volume fraction of 60% is 1;
step three, combining the first filtrate, the second filtrate and the third filtrate prepared in the step two to obtain a saffron crude extraction liquid, and performing supercritical CO treatment on the saffron crude extraction liquid at the temperature of 35 ℃ and under the pressure of 30MPa 2 Inactivating enzyme for 1h by high-pressure carbon dioxide, continuously extracting for 2h by low-pressure reflux at 60 ℃ under the condition of 15-20 kpa, and filtering to obtain saffron essence extract;
and step four, carrying out reduced pressure concentration on the saffron crocus essence extracting solution prepared in the step three, adjusting the pH value to 7.5, and carrying out vacuum drying to obtain the saffron crocus extract.
By adopting the method, 79.89g saffron extract can be obtained from every 1kg saffron.
< example 3>
A stigma croci Sativi extraction process comprises the following steps:
step one, freezing saffron at low temperature, wherein the freezing temperature is below-20 ℃, crushing and grinding the saffron until the particle size is 80 meshes and fine after all saffron are embrittled at low temperature;
step two, adding the saffron powder prepared in the step one into an ethanol solution with the volume fraction of 60%, wherein the material-liquid ratio of the saffron powder to the ethanol solution with the volume fraction of 60% is 1;
step three, combining the first filtrate, the second filtrate and the third filtrate prepared in the step two to obtain a saffron crude extraction liquid, and performing supercritical CO treatment on the saffron crude extraction liquid at the temperature of 35 ℃ under the pressure of 30MPa to obtain the saffron crude extraction liquid 2 Inactivating enzyme with high-pressure carbon dioxide for 1h, continuously extracting under reflux at low pressure for 2h at 60 ℃ under the condition of 15-20 kpa, and filtering to obtain crocus sativus extract;
and step four, carrying out reduced pressure concentration on the saffron crocus essence extracting solution prepared in the step three, adjusting the pH value to 7.0-7.5, and carrying out vacuum drying to obtain the saffron crocus extract.
By adopting the method, 86.47g saffron extract can be obtained from 1kg saffron.
< comparative example >
A stigma croci Sativi extraction process comprises the following steps:
the method comprises the following steps: drying stigma croci in a 45 ℃ oven for 12h, crushing with a high-speed crusher, and sieving with a 40-mesh sieve to obtain stigma croci powder;
step two, adding the saffron powder prepared in the step one into an ethanol solution with the volume fraction of 60%, wherein the material-liquid ratio of the saffron powder to the ethanol solution with the volume fraction of 60% is 1;
step three, adding the first filter residue filtered in the step two into an ethanol solution with the volume fraction of 70%, wherein the material-liquid ratio of the first filter residue to the ethanol solution with the volume fraction of 70% is 1;
step four, adding the second filter residue filtered in the step three into 75% by volume of ethanol solution, wherein the material-liquid ratio of the second filter residue to the 75% by volume of ethanol solution is 1;
and step five, combining the first filtrate, the second filtrate and the third filtrate, concentrating under reduced pressure, adjusting the pH value to 7.0-7.5, and drying in vacuum to obtain the saffron extract.
By adopting the method, 96.13 +/-1.24 g of saffron extract can be obtained per 1kg of saffron.
< determination of content of active ingredient in saffron crocus extract >
1) HPLC analysis of crocin I and crocin II
(1) A chromatographic column: ultimate XB-C18 (4.6 mm × 250mm,5 μm), mobile phase: acetonitrile: water =32 (V: V) (containing 0.1% formic acid). The volume flow is 1.0mL/min, the detection wavelength is 440nm, and the column temperature is 35 ℃;
(2) Preparation of control solutions: accurately weighing 15.0mg of crocin I reference substance and 12.0mg of crocin II reference substance, placing in a 25mL volumetric flask, adding mobile phase liquid for dilution to scale, shaking up to obtain crocin I standard stock solution with concentration of 0.60mg/mL and crocin II standard stock solution with concentration of 0.48mg/mL;
(3) Preparation of a test solution: precisely weighing 1g of stigma croci Sativi extract, adding ethanol to scale, shaking, placing in 100mL brown measuring flask, precisely transferring 2mL of the above solution to 10mL measuring flask, metering to scale with mobile phase, shaking, and filtering with 0.45 μm microporous membrane to obtain sample solution.
Respectively and precisely measuring appropriate amount of reference solution of crocin I, diluting with mobile phase into 5 working solutions with concentration of 15, 30, 60, 150, 300 μ g/mL, and measuring by injecting 10 μ L sample according to the above chromatographic conditions. Respectively and precisely measuring appropriate amount of reference solution of crocin II, diluting with mobile phase into 6 working solutions with concentration of 6, 12, 24, 48, 120, 240 μ g/mL, and measuring by injecting 10 μ L sample according to the above chromatographic conditions. And drawing standard curves of the crocin I and the crocin II by taking the peak area value as an ordinate and taking the sample amount of the reference substance as an abscissa.
The saffron extracts obtained in examples 1 to 3 and comparative example were precisely weighed and prepared into test solution according to the test solution preparation method, 5 parts of each example were taken, the sample amount was 10 μ L according to the chromatographic condition, and the average content of crocin i and crocin ii in the saffron extract was calculated, respectively, and the results are shown in table 1.
TABLE 1
Example 1 Example 2 Example 3 Comparative example
Crocin I 47% 51% 52% 33
Crocin II
16% 13% 15% 8%
The amounts of crocin I and crocin II extracted from saffron starting material were calculated from the data in Table 1 and the results are shown in Table 2:
TABLE 2
Figure BDA0003819971380000071
As can be seen from table 2, although the saffron extract quality of the comparative examples was higher than that of examples 1 to 3, the amounts of crocin I and crocin II, which are effective ingredients in the saffron extract, were still lower than those of examples 1 to 3.
2) HPLC analysis of flavonols
(1) A chromatographic column: diamonsil C18 (4.6 mm. Times.150mm, 5 μm), mobile phase: 0-4% methanol: phosphoric acid = (60: 1mL/min, detection wavelength: 365nm, column temperature: 25 ℃, sample introduction: 10 μ L.
(2) Preparation of control solutions: accurately weighing quercetin reference substance, and preparing 0.24mg/mL reference substance stock solution with methanol as solvent. 0.5mL of the stock solution was taken in a 10mL measuring flask, dissolved and diluted to the mark with methanol, and shaken up to serve as a control solution.
(3) Preparation of a test solution: precisely weighing 1g of stigma croci Sativi extract, adding methanol to scale, shaking, placing in 100mL brown measuring flask, precisely transferring 2mL of the above solution to 10mL measuring flask, metering to scale with mobile phase, shaking, and filtering with 0.45 μm microporous membrane to obtain test solution.
Respectively and precisely measuring a proper amount of a standard solution of a quercetin reference substance, diluting the standard solution into 6 working solutions with the concentrations of 3, 6, 9, 12, 15 and 18 mu g/mL by using a mobile phase, and respectively injecting 10 mu L of the working solutions according to the chromatographic conditions for measurement. And drawing a standard curve of the quercetin by taking the peak area value as a vertical coordinate and taking the sample amount of the reference substance as a horizontal coordinate.
Precisely weighing the saffron extracts obtained in the examples 1 to 3 and the comparative example, preparing a sample solution according to a sample solution preparation method, taking 5 parts of each example, detecting according to chromatographic conditions, wherein the sample amount is 10 mu L, and respectively calculating the average content of quercetin in the saffron extracts, wherein the results are shown in Table 3.
TABLE 3
Example 1 Example 2 Example 3 Comparative example
Quercetin
13% 14% 15% 6%
The extraction amount of quercetin from saffron raw material can be calculated according to the data in table 3, and the result is shown in table 4:
TABLE 4
Example 1 Example 2 Example 3 Comparative example
Quercetin (mg/g) 10.83 11.18 12.97 5.77
As can be seen from table 4, although the saffron extract of the comparative example has higher quality than examples 1 to 3, the extraction amount of quercetin, which is an active ingredient in the saffron extract, is still lower than examples 1 to 3.
< example 4>
The implementation process of the saffron extraction process is basically the same as that of the embodiment 3, except that the low-pressure reflux extraction process in the step three is carried out by using the saffron extraction device of the embodiment, as shown in fig. 1, the saffron extraction device comprises:
the heating tank 1 is characterized in that a water adding pipe 2 is arranged on the wall of the heating tank 1, a water discharging pipe 3 is arranged at the bottom of the heating tank 1, a first valve 4 is arranged at the orifice of the water discharging pipe 3, and an electric heating coil pipe 5 is further arranged in the heating tank 1;
the material tank 6 is arranged in the heating tank 1, the electric heating coil pipe 5 surrounds the material tank 6, a charging pipe 7 is arranged on the wall of the material tank 6, the charging pipe 7 penetrates out of the wall of the heating tank 1, a second valve 8 is arranged at the orifice of the charging pipe 7, a steam pipe 9 is arranged at the top of the material tank 6, and the steam pipe 9 penetrates out of the top of the heating tank 1;
the condenser comprises a conical container 10, a plurality of condensing pipes 11, a condensing tank 12 and a cooling water tank 13, wherein the top of the conical container 10 is connected with a steam pipe 9 penetrating out of the top of the heating tank 1, the bottom of the conical container 10 is connected with the plurality of condensing pipes 11 in parallel, the bottoms of the plurality of condensing pipes 11 are connected with the top of the condensing tank 12, the bottom of the condensing tank 12 is higher than the liquid level of the material in the material tank 6, the conical container 10, the plurality of condensing pipes 11 and the condensing tank 12 are all arranged in the cooling water tank 13, a water outlet 14 is formed in the upper part of the wall of the cooling water tank 13, and a water inlet 15 is formed in the lower part of the wall of the cooling water tank 13;
the bottom of the condensing tank 12 is provided with a return pipe 16, the return pipe 16 penetrates out of the wall of the cooling water tank 13 and penetrates into the heating tank 1 and is connected with the bottom of the material tank 6, the heating tank 1 is also provided with a vacuum pump 17, the vacuum pump 17 is connected with an air suction pipe 18, the air suction pipe 18 penetrates into the heating tank 1 and is communicated with the material tank 6, and the air suction pipe 18 is provided with a third valve 19.
The usage process of the saffron extraction device comprises the following steps: firstly, a crude saffron extraction liquid after enzyme deactivation is added into the material tank 6 through a feeding pipe 7, clear water higher than the liquid level of the crude saffron extraction liquid is injected into a heating tank 1 through a water adding pipe 2, then cooling water is filled into a cooling water tank 13 through a water inlet 15, when the liquid level of the cooling water in the cooling water tank 13 is higher than that of a conical container 10, the cooling water can be discharged from a water outlet 14 at the upper part of the cooling water tank 13, and enters a cooling tower for recycling through the water inlet 15 of the cooling water tank 13. Secondly, the second valve 8 is closed, at this time, the material tank 6, the steam pipe 9, the conical container 10, the condensation pipe 11, the condensation tank 12 and the return pipe 16 form a closed communication space, the vacuum pump 17 is started to suck air in the closed communication space to reduce the air pressure to below 5kpa, the vacuum pump 17 and the third valve 19 are closed, then the clear water in the heating tank 1 is heated through the electric heating coil 5 to ensure that the water temperature reaches about 50 ℃, the crude saffron extraction liquid starts boiling evaporation due to the low-pressure environment in the material tank 6, the evaporation gas enters the condenser along the steam pipe 9 to ensure that the air pressure in the closed communication space gradually rises, the evaporation gas is condensed in the condenser to form condensate liquid, the air pressure is reduced, when the water temperature slowly rises to about 60 ℃, the increased air pressure of the crude saffron extraction liquid is heated and evaporated to ensure that the increased air pressure of the closed communication space is dynamically balanced with the reduced air pressure of the steam in the condenser, the air pressure in the closed communication space is maintained at about 15-20 kpa, and the cooling liquid in the condensation tank 12 can continuously return from the return pipe 16 to the material tank 6 to form a continuous low-pressure reflux extraction process based on the principle of the communicating vessel.
In this embodiment the saffron extraction element has realized the continuous low pressure backward flow that is suitable for on the industrial production for the first time and has drawed, and the high temperature oxidation of active ingredient decomposes in the medicinal material when having avoided the ordinary pressure backward flow to draw, and production efficiency is high, and it is effectual to purify.
More preferably, the bottom of the material tank 6 is provided with an extract discharging pipe 20, the extract discharging pipe 20 penetrates out of the bottom of the heating tank 1, and a fourth valve 21 is arranged at the orifice of the extract discharging pipe 20. In the use process of this embodiment, when the crude saffron extraction liquid is added into the material tank 6, the fourth valve 21 needs to be closed first, and when the extraction process is finished, the fourth valve 21 can be opened to discharge the purified refined saffron extraction liquid from the extraction liquid discharge pipe 20.
It is more preferable that a three-way joint is provided between the return pipe 16 and the condensation tank 12, one end of the three-way joint is connected to the bottom of the condensation tank 12, the other end is connected to the return pipe 16, the third end is connected to a solvent discharge pipe 22, the solvent discharge pipe 22 is extended from the bottom of the cooling water tank 13, and a fifth valve 23 is provided at the nozzle of the solvent discharge pipe 22.
Preferably, the return line 16 is provided with a sixth valve 24.
Thus, the present embodiment can complete the decompression and concentration operation on the saffron crocus extraction device, and the specific process comprises: when the extraction in the material pipe is finished and only the saffron extract is left, the sixth valve 24 is closed, the material tank 6 is continuously heated, the saffron extract contained in the material tank 6 is boiled and evaporated, the evaporated gas enters the condenser through the steam pipe 9, condensate is formed in the condensation tank 12, the condensate cannot return to the material tank 6 along the return pipe 16 due to the closing of the sixth valve 24, the pressure reduction and concentration process is carried out in the material tank 6 at the moment, after the concentration is finished, the third valve 19 on the exhaust pipe 18 is opened, the interior of the material tank 6 returns to the normal pressure, the fifth valve 23 is opened, the solvent condensate in the condensation tank 12 can be discharged, and the concentrated solution in the material tank 6 can be discharged from the extract discharge pipe 20. This embodiment saffron extraction element can not only realize that continuous low pressure backward flow draws, can also carry out the decompression concentration, and a tractor serves several purposes has practiced thrift manufacturing cost, has reduced material transfer process, has improved production efficiency.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.

Claims (9)

1. The saffron crocus extraction process is characterized by comprising the following steps:
step one, freezing saffron at low temperature, wherein the freezing temperature is below-20 ℃, crushing and grinding the saffron until the particle size is 80 meshes and fine after all saffron are embrittled at low temperature;
step two, adding the saffron crocus powder prepared in the step one into an ethanol solution with the volume fraction of 60%, carrying out low-temperature ultrasonic extraction for 2-3 h at the temperature of 0-4 ℃, filtering to obtain a first filtrate, adding the filtered first filter residue into the ethanol solution with the volume fraction of 70%, carrying out low-temperature ultrasonic extraction for 1-1.5 h at the temperature of 0-4 ℃, filtering to obtain a second filtrate, adding the filtered second filter residue into the ethanol solution with the volume fraction of 75%, carrying out low-temperature ultrasonic extraction for 30-40 min at the temperature of 0-4 ℃, and filtering to obtain a third filtrate;
step three, combining the first filtrate, the second filtrate and the third filtrate prepared in the step two to obtain a saffron crude extraction liquid, inactivating enzyme by adopting high-pressure carbon dioxide, continuously performing low-pressure reflux extraction for 2 hours at 60 ℃ and under the condition of 15-20 kpa, and filtering to obtain a saffron crocus essence extracting solution;
and step four, carrying out reduced pressure concentration on the saffron crocus essence extracting solution prepared in the step three, adjusting the pH value to 7.0-7.5, and carrying out vacuum drying to obtain the saffron crocus extract.
2. The saffron extraction process according to claim 1, wherein in the second step, the ratio of saffron powder to 60% by volume of ethanol solution is 1.
3. The saffron crocus extraction process according to claim 1, wherein the ultrasonic power used for low temperature ultrasonic extraction in the second step is 500W, and the circulating cooling water is adopted to maintain the ethanol solution at 0-4 ℃ in the low temperature ultrasonic extraction process.
4. The saffron extraction process according to claim 1, wherein the crude saffron extract is extracted by supercritical CO at 30MPa and 35 deg.C 2 Inactivating enzyme with high pressure carbon dioxide for 1 hr.
5. The saffron extraction process according to claim 1, wherein said saffron extract is used to make granules, tablets or capsules.
6. A saffron extraction device, characterized in that it is used in the low-pressure reflux extraction process in step three of the saffron extraction process of claim 1, said saffron extraction device comprises:
the heating tank is provided with a water feeding pipe on the wall, a water discharging pipe is arranged at the bottom of the heating tank, a first valve is arranged at the orifice of the water discharging pipe, and an electric heating coil pipe is also arranged in the heating tank;
the material tank is arranged in the heating tank, the electric heating coil pipe surrounds the material tank, a charging pipe is arranged on the wall of the material tank, the charging pipe penetrates out of the wall of the heating tank, a second valve is arranged at the opening of the charging pipe, a steam pipe is arranged at the top of the material tank, and the steam pipe penetrates out of the top of the heating tank;
the condenser comprises a conical container, a plurality of condensing pipes, a condensing tank and a cooling water tank, wherein the top of the conical container is connected with a steam pipe penetrating out of the top of the heating tank, the bottom of the conical container is connected with the plurality of condensing pipes in parallel, the bottoms of the plurality of condensing pipes are connected with the top of the condensing tank, the bottom of the condensing tank is higher than the liquid level of materials in the material tank, the conical container, the plurality of condensing pipes and the condensing tank are all arranged in the cooling water tank, a water outlet is formed in the upper part of the wall of the cooling water tank, and a water inlet is formed in the lower part of the wall of the cooling water tank;
the bottom of the condensing tank is provided with a return pipe, the return pipe penetrates out of the wall of the cooling water tank and penetrates into the heating tank to be connected with the bottom of the material tank, a vacuum pump is further arranged outside the heating tank and connected with an exhaust pipe, the exhaust pipe penetrates into the heating tank to be communicated with the material tank, and a third valve is arranged on the exhaust pipe.
7. The saffron extraction device according to claim 6, wherein said material tank is provided at its bottom with an extract discharge tube, said extract discharge tube extending out of said heating tank bottom, said extract discharge tube having a nozzle provided with a fourth valve.
8. The saffron crocus extraction device according to claim 6, wherein a tee joint is provided between said return pipe and said condensation tank, one end of said tee joint is connected to the bottom of said condensation tank, the other end is connected to said return pipe, the third end is connected to a solvent discharge pipe, said solvent discharge pipe passes through the bottom of said cooling water tank, and a fifth valve is provided at the mouth of said solvent discharge pipe.
9. The saffron extraction device according to claim 6, wherein said return line is provided with a sixth valve.
CN202211038798.XA 2022-08-29 2022-08-29 Saffron extraction process and device Pending CN115261142A (en)

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CN209193848U (en) * 2018-10-25 2019-08-02 宜昌玫园生物科技有限公司 Crocin high-efficiency device for extracting in a kind of cape jasmine fruit
CN111084795A (en) * 2019-09-12 2020-05-01 天津芸熙生物技术有限公司 Preparation process of compound preparation extracted from sandalwood leaves at low temperature
CN111973532A (en) * 2020-09-09 2020-11-24 广州科盈化妆品有限公司 Saffron extract for treating skin acne and application thereof
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* Cited by examiner, † Cited by third party
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KR20020046393A (en) * 2000-12-13 2002-06-21 윤승열 Extraction Apparatus For Essential Terpene-oil
KR20140021418A (en) * 2012-08-10 2014-02-20 주식회사 영일이엔지 Vacuum low temperature extraction apparatus for producing indigo pigment
CN105287677A (en) * 2015-11-27 2016-02-03 江西京通美联药业有限公司 Method for extracting and further processing ainsliaea fragrans total flavonoid
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