CN119701405A - A kind of ginger extract and refining method thereof - Google Patents
A kind of ginger extract and refining method thereof Download PDFInfo
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Abstract
本发明涉及提取物精制技术领域，具体公开了一种生姜提取物及其精制方法。本发明的精制生姜提取物的方法，其包括：（1）采用低碳醇分散溶解生姜提取物原料，获得料液一；所述生姜提取物原料为采用超临界二氧化碳萃取生姜获得的生姜提取物；（2）将所述料液一的pH值调节为12‑13，充分反应后，再将pH值调节至5‑6，获得料液二；（3）将所述料液二浓缩至低碳醇的浓度为15%‑45%后，静置，分离获得下层物料；（4）将所述下层物料与浓度为15%‑45%的低碳醇充分混合后，静置，分离收集下层。本发明的方法可有效去除生姜提取物原料中的农残，获得更加安全的产品。The present invention relates to the technical field of extract refining, and specifically discloses a ginger extract and a refining method thereof. The method for refining ginger extract of the present invention comprises: (1) using low-carbon alcohol to disperse and dissolve ginger extract raw materials to obtain liquid one; the ginger extract raw material is ginger extract obtained by extracting ginger with supercritical carbon dioxide; (2) adjusting the pH value of liquid one to 12-13, and after sufficient reaction, adjusting the pH value to 5-6 to obtain liquid two; (3) concentrating liquid two to a concentration of low-carbon alcohol of 15%-45%, standing, separating and obtaining a lower layer material; (4) fully mixing the lower layer material with a low-carbon alcohol with a concentration of 15%-45%, standing, and separating and collecting the lower layer. The method of the present invention can effectively remove agricultural residues in the raw material of ginger extract and obtain a safer product.
Description
Technical Field
The invention relates to the technical field of extract refining, in particular to a ginger extract and a refining method thereof.
Background
Ginger is a fresh rhizome of perennial herb of the genus zingiberaceae. The ginger is warm in nature, and the special gingerol can stimulate gastrointestinal mucosa, so that the gastrointestinal congestion and digestion capacity are enhanced, and the ginger can effectively treat abdominal distension, abdominal pain, diarrhea, vomiting and the like caused by excessive eating of cold and cool food. After eating ginger, people feel that the body is hot, because the ginger can dilate blood vessels, quicken blood circulation and promote pores on the body to open, so that not only can the superfluous heat be carried away, but also germs and cold in the body can be carried out.
The extraction method of the ginger extract mainly comprises a steam distillation method, a solvent extraction method, an ultrasonic method, a supercritical carbon dioxide extraction method and a squeezing method at present, the supercritical carbon dioxide extraction technology at the present stage is mature, the extraction temperature in the supercritical carbon dioxide extraction process is low, the yields of ginger essential oil and gingerol in the extraction process are ideal, and the method is very suitable for large-scale ginger raw material treatment and industrial production.
However, in order to maximize the yield of ginger, the excessive pesticide is usually used for fumigation treatment on the planting area before planting to prevent insect erosion and virus infection, the intermittent pesticide spraying is needed in the planting process to prevent insects, the healthy growth of ginger seedlings is ensured, and a large amount of pesticide needs to be sprayed for antibiosis and insect prevention in the storage process after harvesting. This results in the problem of exceeding pesticide residues in the produced ginger. When the extraction is performed through supercritical carbon dioxide extraction, part of pesticide residues in the ginger raw material can migrate into a ginger extract product, and the types of the pesticide residues are complex, various in properties and overdetermined in dosage, wherein the main pesticide residue types comprise organophosphorus pesticide residues, organochlorine pesticide residues and the like, and the pesticide residues are one of the main factors for limiting the application of the ginger extract in foods.
At present, related preparation technology related to pesticide residue removal relates to separation by using supercritical carbon dioxide extraction technology, for example, chinese patent CN116474415A uses ginger essential oil as entrainer to separate pesticide residue in ginger oleoresin, but the operation is complex, and the effect of removing pesticide residue still needs to be improved. Therefore, further research on the problem of pesticide residue removal of ginger extract is required.
Disclosure of Invention
The present invention provides a method for purifying ginger extract with low pesticide residue and high yield.
The invention provides a method for refining ginger extract, which comprises the following steps:
(1) Dispersing and dissolving raw ginger extract raw materials by adopting low-carbon alcohol to obtain a first feed liquid, wherein the raw ginger extract raw materials are ginger extracts obtained by extracting ginger by adopting supercritical carbon dioxide;
(2) The pH value of the feed liquid I is adjusted to be 12-13, and after full reaction, the pH value is adjusted to be 5-6, so that feed liquid II is obtained;
(3) Concentrating the feed liquid II until the concentration of the low-carbon alcohol is 15% -45%, standing at 30-50 ℃, and separating to obtain a lower layer material (oily resin);
(4) And (3) fully mixing the lower layer material with low-carbon alcohol with the concentration of 15% -45%, standing at 30-50 ℃, and collecting the lower layer.
According to the research, the problem of pesticide residues in the ginger extract obtained by extracting the ginger by using the supercritical carbon dioxide is serious, and the application requirements cannot be met, and further, according to the research, the thiamethoxam and fosthiazate can be effectively removed after the ginger extract obtained by extracting the ginger by using the supercritical carbon dioxide is firstly dissolved and dispersed and then the pH value of the ginger extract is adjusted to a specific alkaline condition for full reaction. And then adjusting the pH value of the feed liquid to 5-6, and then purifying and washing the feed liquid at a specific temperature to further remove other pesticide residues, so as to finally obtain the ginger extract with low pesticide residues.
If the pH value of the feed liquid is not within the limit of the invention when the feed liquid is fully reacted under alkaline conditions, the sufficient removal of pesticide residues and the high yield of gingerol in the product cannot be achieved. If the concentration of the alcohol solution is too low or the temperature is too low during purification and washing, the sufficient removal of pesticide residues is not facilitated, and if the concentration of the alcohol solution is too high or the temperature is too high, the yield of gingerol in the product is affected. The purification and washing conditions defined by the invention can be favorable for improving the yield of gingerol.
Compared with the traditional pesticide residue removing method, the method provided by the invention has the advantages of being safer, more green, low in production cost and suitable for industrial mass production, and the obtained ginger extract has high gingerol purity and can be used with high value.
The raw materials of the ginger extract can be produced by a supercritical carbon dioxide extraction method known in the art, for example, the specific production method comprises the steps of crushing dried ginger slices, putting the crushed dried ginger slices into a supercritical carbon dioxide extraction kettle, raising the pressure of the extraction kettle to 25-30MPa, keeping the temperature to 35-55 ℃, enabling the flow of carbon dioxide to be 5-10kg/h per kilogram of dried ginger raw material, extracting for 3-5h, enabling the pressure of a separation kettle to be 6-10MPa, and enabling the temperature of the separation kettle to be 30-50 ℃.
Wherein the pesticide residue comprises one or more of organophosphorus pesticide, organochlorine pesticide and phenylamide pesticide. Wherein the organophosphorus pesticides include thiamethoxam, imidacloprid, fosthiazate, clothianidin and the like, the organochlorine pesticides include chlorpyrifos and the like, and the phenylamide pesticides include metalaxyl and the like.
In the present invention, an acid-base reagent such as sodium hydroxide, potassium hydroxide, hydrochloric acid, phosphoric acid or nitric acid is used for adjusting the pH, and sodium hydroxide and hydrochloric acid are preferably used.
In the method step (1), the low-carbon alcohol is one or more of ethanol and methanol, and the concentration of the low-carbon alcohol is more than or equal to 55%, preferably 55% -95%.
Further preferably, the lower alcohol is ethanol, and the concentration of the lower alcohol is 65%.
The invention preferably uses an aqueous ethanol solution to facilitate industrial recycling.
In the method of the invention, the mass volume ratio of the raw ginger extract to the low-carbon alcohol is 1 (3-7) g/mL, and/or the dispersing and dissolving in the step (1) are carried out at 25-50 ℃.
Preferably, the mass volume ratio of the raw materials of the ginger extract and the low-carbon alcohol is 1:4 g/mL, and the dispersing and dissolving are carried out at 30-50 ℃ and preferably at 35-45 ℃.
In the method step (4), the mass volume ratio of the lower material to the low-carbon alcohol is 1 (1-3) g/mL.
In the method step (2), the full reaction is carried out at 25-55 ℃ for 1-3 hours.
Preferably, in step (2), the complete reaction is carried out at 30-50 ℃ (more preferably 35-45 ℃). The reaction is carried out under the condition of the invention, which not only can ensure the full progress of the reaction, but also is beneficial to avoiding the loss of the yield of gingerol.
After step (4) of the method of the invention, the method also comprises a step of removing solvent residues.
The conditions for removing the solvent residue can be water bath temperature of 55-70 ℃ and vacuum degree of-0.06 MPa to-0.1 MPa.
In the method step (3), the concentration condition is that the water bath temperature is 55-70 ℃ and the vacuum degree is-0.06 MPa to-0.1 MPa.
In the method of the present invention, it is preferable to repeat the step (4) 2 to 5 times, more preferably 2 to 3 times, so as to achieve both the effect of removing pesticide residues and the production efficiency.
The invention also provides a ginger extract, which is prepared by the method.
The ginger extract obtained by the method has low pesticide residues, and pesticide residues such as thiamethoxam, fosthiazate, chlorpyrifos, metalaxyl and the like are not detected (the detection limit is 0.1 ppm).
The invention has the advantages that:
The invention provides a method for removing pesticide residues in ginger extract, solves the problem of exceeding pesticide residues in ginger extract products, has simple process operation and low cost, can be effectively applied to large-scale production, and can thoroughly separate gingerol from pesticide residues to prepare clean and safe ginger extract products.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention may be made by those skilled in the art without departing from the spirit and scope of this invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents and the like used in the examples below, unless otherwise indicated, are all those available commercially or may be prepared by methods conventional in the art.
The raw materials used in the embodiment of the invention are ginger extract produced by adopting a supercritical carbon dioxide extraction method for extracting gingerol, and the specific production method comprises the steps of crushing dried ginger slices, putting the crushed dried ginger slices into a supercritical carbon dioxide extraction kettle, raising the pressure of the extraction kettle to 28MPa, keeping the temperature at 45 ℃, enabling the carbon dioxide flow to be 8kg/h per kilogram of dried ginger raw material, enabling the extraction time to be 4h, enabling the pressure of a separation kettle to be 8MPa, and enabling the temperature of the separation kettle to be 40 ℃.
The final ginger extract contains gingerol (including 6-gingerol, 8-gingerol, 10-gingerol, 6-shogaol, 8-shogaol) 41.35%, chlorpyrifos 2.13ppm, thiamethoxam 3.73ppm, imidacloprid 2.46ppm, fosthiazate 1.72ppm, metalaxyl 6.25ppm.
In the invention, chlorpyrifos, fosthiazate and metalaxyl are detected by referring to GB 23200.113, thiamethoxam is detected by referring to GB23200.9, and imidacloprid is detected by referring to GB/T20769.
Example 1
The embodiment provides a method for removing pesticide residues in ginger extract, which comprises the following specific steps:
1. Weighing 100kg of ginger extract raw material, adding ethanol solution (concentration 65%) with the volume (L) 4 times of the weight of the extract, stirring at 40 ℃ for 0.5h, and fully mixing to obtain feed liquid I;
2. Adding a sodium hydroxide reagent into the feed liquid I, adjusting the pH value to be 12.5, stirring and reacting for 2 hours at 40 ℃, then adding a hydrochloric acid diluent into the feed liquid, and adjusting the pH value to be 5.5 to obtain a feed liquid II;
3. Concentrating the second feed liquid at 65 ℃ and a vacuum degree of-0.08 MPa until the concentration of ethanol in the feed liquid is 30%, standing for 0.5h at 40 ℃, and collecting the lower layer;
4. Adding 30% ethanol solution (feed-liquid ratio 1:2 kg/L) into the lower material again, stirring at 40deg.C for 1 hr, standing for 0.5 hr, and collecting the lower material. Repeating ethanol solvent washing according to the above operation, washing for 3 times, combining the upper ethanol solutions after washing for 3 times, respectively desolventizing residues of the combined upper ethanol solution and lower material (water bath temperature is 65 ℃ and vacuum degree is-0.08 MPa), concentrating the lower layer to obtain 86.69kg of pesticide residue removing ginger oleoresin, controlling the content of gingerol to 39.87%, controlling the content yield to 83.59%, controlling the content of chlorpyrifos, thiamethoxam, imidacloprid, fosthiazate and metalaxyl to be undetected (detection limit to 0.1 ppm), concentrating the ethanol solution to obtain 12.43kg of common ginger oleoresin, controlling the content of gingerol to 41.43%, controlling the content yield to 12.45%, controlling the content of chlorpyrifos to 2.81ppm, controlling the content of imidacloprid to 3.47ppm, controlling the content of metalaxyl to 10.84ppm, controlling the content of thiamethoxam and fos to be undetected (detection limit to 0.1 ppm), and controlling the total content of gingerol to 96.04%.
Example 2
The embodiment provides a method for removing pesticide residues in ginger extract, which comprises the following specific steps:
1. Weighing 100kg of ginger extract raw material, adding ethanol solution (concentration 55%) with the volume (L) 7 times of the weight of the extract, stirring at 50 ℃ for 0.5h, and fully mixing to obtain feed liquid I;
2. Adding a sodium hydroxide reagent into the feed liquid I, adjusting the pH value to be 12.0, stirring and reacting for 3 hours at 55 ℃, then adding a hydrochloric acid diluent into the feed liquid, and adjusting the pH value to be 5 to obtain a feed liquid II;
3. Concentrating the second feed liquid at 70 ℃ and 0.06MPa to 15% of ethanol concentration in the feed liquid, standing at 50 ℃ for 0.5h, and collecting the lower layer;
4. Adding 15% ethanol solution (feed-liquid ratio 1:3 kg/L) into the lower material again, stirring at 50deg.C for 1h, standing for 0.5h, and collecting the lower material. Repeating ethanol solvent washing according to the above operation, washing for 5 times, combining the upper ethanol solutions after washing for 5 times, respectively desolventizing residues of the combined upper ethanol solution and lower material (water bath temperature is 70 ℃, vacuum degree is-0.06 MPa), concentrating the lower layer to obtain 86.82kg of pesticide residue removing ginger oleoresin, 40.03% of gingerol content, 84.05% of content yield, namely chlorpyrifos, thiamethoxam, imidacloprid, fosthiazate and metalaxyl, wherein the detection limit is 0.1ppm, concentrating the ethanol solution to obtain 12.14kg of common ginger oleoresin, 41.12% of gingerol content, 12.07% of content yield, 2.45ppm of chlorpyrifos, 3.45ppm of imidacloprid, 9.74ppm of metalaxyl, undetected thiamethoxam and fosthiazate (detection limit is 0.1 ppm), and 96.12% of total content yield of gingerol.
Example 3
The embodiment provides a method for removing pesticide residues in ginger extract, which comprises the following specific steps:
1. Weighing 100kg of ginger extract raw material, adding ethanol solution (concentration 95%) with the volume (L) 3 times of the weight of the extract, stirring at 25 ℃ for 0.5h, and fully mixing to obtain feed liquid I;
2. Adding a sodium hydroxide reagent into the feed liquid I, adjusting the pH value to be 13.0, stirring and reacting for 1h at 25 ℃, then adding a hydrochloric acid diluent into the feed liquid, and adjusting the pH value to be 6 to obtain a feed liquid II;
3. concentrating the second feed liquid at the water bath temperature of 55 ℃ and the vacuum degree of-0.1 MPa until the concentration of ethanol in the feed liquid is 45%, standing for 0.5h at the temperature of 30 ℃, and collecting the lower layer;
4. Adding 45% ethanol solution (feed-liquid ratio 1:1 kg/L) into the lower material again, stirring at 30deg.C for 1h, standing for 0.5h, and collecting the lower material. Repeating ethanol solvent washing according to the above operation, washing for 2 times, combining the upper ethanol solutions after washing for 2 times, respectively desolventizing residues of the combined upper ethanol solution and lower materials (water bath temperature is 55 ℃, vacuum degree is-0.1 MPa), concentrating the lower layer to obtain 85.46kg of pesticide residue removing ginger oleoresin, 39.68% of gingerol content and 82.01% of content yield, wherein no detection (detection limit of 0.1 ppm) is carried out on chlorpyrifos, thiamethoxam, imidacloprid, fosthiazate and metalaxyl, 12.76kg of common ginger oleoresin is obtained after concentrating the ethanol solution, the gingerol content is 42.35%, the content yield is 13.07%, the chlorpyrifos content is 3.21ppm, the imidacloprid content is 3.97ppm, the metalaxyl content is 11.23ppm, the thiamethoxam and fos are undetected (detection limit of 0.1 ppm), and the total content yield of gingerol is 95.08%.
Comparative example 1
This comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as example 1, except that in step 2, sodium hydroxide reagent is added to feed liquid one, ph=14 is adjusted, and the rest steps are the same as example 1. And finally, concentrating the lower layer to obtain 86.61kg of pesticide residue removed ginger oleoresin, wherein the content of gingerol is 23.17%, the content yield is 48.53%, all chlorpyrifos, thiamethoxam, imidacloprid, fosthiazate and metalaxyl are not detected (the detection limit is 0.1 ppm), and 12.46kg of common ginger oleoresin is obtained after concentrating the ethanol solution, the content of gingerol is 24.15%, the chlorpyrifos is 0.41ppm, the imidacloprid is 0.35ppm, the metalaxyl is 0.48ppm, the thiamethoxam and fosthiazate are not detected (the detection limit is 0.1 ppm), and the content yield is 7.28%. The total content yield of gingerol is 55.81%.
Comparative example 2
This comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as example 1, except that in step 2, a sodium hydroxide reagent is added to feed liquid one, and ph=11 is adjusted. And concentrating the lower layer to obtain 86.72kg of ginger oleoresin without pesticide residues, wherein the ginger peppery content is 40.56%, the content yield is 85.06%, chlorpyrifos is 1.31ppm, thiamethoxam is 0.27ppm, imidacloprid is 0.73ppm, fosthiazate is 0.11ppm, metalaxyl is 1.97ppm, and the ethanol solution is concentrated to obtain 12.38kg of common ginger oleoresin, the ginger peppery content is 41.96%, the content yield is 12.56%, chlorpyrifos is 5.42ppm, thiamethoxam is 1.17ppm, imidacloprid is 4.38ppm, fosthiazate is 0.89ppm and metalaxyl is 28.36ppm. The total content yield of gingerol is 97.63%.
Comparative example 3
This comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as example 1, except that the second feed solution obtained in step 2 is directly concentrated to remove pesticide residues, and the ethanol separation and washing steps in steps 3 and 4 are not performed. Finally, 99.87kg of pesticide residue removed ginger oleoresin is obtained, the gingerol content is 39.92%, the content yield is 96.42%, chlorpyrifos is 0.16ppm, thiamethoxam is not detected, imidacloprid is 0.39ppm, fosthiazate is not detected, and metalaxyl is 0.48ppm.
Comparative example 4
The comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as that of example 1, except that steps 1,2 and 3 are not performed, and raw ginger extract is directly added with 30% ethanol to be washed for 4 times (feed-liquid ratio is 1:2 kg/L). And finally, concentrating the lower layer to obtain 86.43kg of ginger oleoresin without pesticide residues, wherein the ginger peppery content is 40.97%, the content yield is 85.64%, chlorpyrifos is 1.43ppm, thiamethoxam is 0.75ppm, imidacloprid is 1.33ppm, fosthiazate is 0.42ppm, metalaxyl is 2.52ppm, and the ethanol solution is concentrated to obtain 12.53kg of common ginger oleoresin, the ginger peppery content is 42.76%, the content yield is 12.96%, chlorpyrifos is 7.08ppm, thiamethoxam is 24.62ppm, imidacloprid is 10.65ppm, fosthiazate is 10.87ppm and metalaxyl is 31.37ppm. The yield of the total gingerol content is 98.59%.
Comparative example 5
The comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as that of example 1, except that in step 3, the second feed liquid is concentrated to an ethanol content of <1%, and the lower ginger oleoresin is washed with 30% ethanol for 4 times, and the detailed steps are not the same as those of example 1. And finally, concentrating the lower layer to obtain 86.53kg of pesticide residue removed ginger oleoresin, wherein the content of gingerol is 39.85%, the content yield is 83.39%, chlorpyrifos is 0.12ppm, thiamethoxam is not detected, imidacloprid is 0.11ppm, fosthiazate is not detected, metalaxyl is 0.15ppm, the ethanol solution is concentrated to obtain 12.28kg of common ginger oleoresin, the content of gingerol is 41.41%, the content yield is 12.30%, chlorpyrifos is 1.74ppm, imidacloprid is 2.84ppm, metalaxyl is 9.97ppm, thiamethoxam and fosthiazate are not detected (the detection limit is 0.1 ppm), and the total content yield of gingerol is 95.69%.
Comparative example 6
The comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as that of example 1, except that in step 3, the second feed liquid is concentrated to a concentration of 10% of ethanol in the feed liquid, and the feed liquid is left to stand for 0.5h at 40 ℃ to collect the lower layer, and in step 4, the ethanol solution with the concentration of 10% is added to the lower layer material again for washing, and the rest steps are the same as that of example 1. And finally, concentrating the lower layer to obtain 93.24kg of pesticide residue removed ginger oleoresin, wherein the content of gingerol is 39.74%, the content yield is 89.61%, chlorpyrifos is 0.17ppm, thiamethoxam is not detected, imidacloprid is 0.28ppm, fosthiazate is not detected, metalaxyl is 0.21ppm, the ethanol solution is concentrated to obtain 6.45kg of common ginger oleoresin, the content of gingerol is 39.85%, the content yield is 6.22%, chlorpyrifos is 1.32ppm, imidacloprid is 1.45ppm, metalaxyl is 3.27ppm, thiamethoxam and fosthiazate are not detected (the detection limit is 0.1 ppm), and the total content yield of gingerol is 95.83%.
Comparative example 7
The comparative example provides a method for removing pesticide residues in ginger extract, which is basically the same as that of example 1, except that in step 3, the second feed liquid is concentrated to a concentration of 50% of ethanol in the feed liquid, and the feed liquid is left to stand for 0.5h at 40 ℃ to collect the lower layer, and in step 4, the ethanol solution with the concentration of 50% is added to the lower layer material again for washing, and the rest steps are the same as that of example 1. Finally, 57.32kg of pesticide residue removed ginger oleoresin is obtained after the lower layer is concentrated, 31.54% of gingerol content, 43.72% of content yield, chlorpyrifos, thiamethoxam, imidacloprid, fosthiazate and metalaxyl are not detected, 42.45kg of common ginger oleoresin is obtained after the ethanol solution is concentrated, 51.03% of gingerol content, 52.39% of content yield, 0.89ppm of chlorpyrifos, 0.73ppm of imidacloprid, 2.51ppm of metalaxyl, no detection (detection limit of 0.1 ppm) of thiamethoxam and fosthiazate are detected, and 96.11% of total content of gingerol.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
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| CN119112966A (en) * | 2024-09-13 | 2024-12-13 | 江西海富生物工程有限公司 | A method for producing low-pesticide residue ginseng stem and leaf extract |
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