CN115403457B - A method for preparing Curcuma rhizome extract - Google Patents
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Abstract
The invention provides a preparation method of turmeric extract, which omits the step of petroleum ether extraction and degreasing, and the turmeric medicinal material is baked before extraction, so that volatile oil in turmeric can be removed, the volatile oil removal effect is obvious, and the separation of curcumin compounds and volatile oil is realized, thereby being beneficial to the drying of turmeric extract; in addition, petroleum ether degreasing is not needed, so that the whole extraction process is safer and more environment-friendly; 2) Compared with the prior art, the method omits 2 times of ethanol crystallization steps, and directly crystallizes in the cold storage and standing stage, and the yield of the turmeric extract is not affected; 3) The test result shows that the curcumin content in the turmeric extract is 55.4-57.3%, the curcumin compound content is 66.3-69.1%, the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin is 64.3-67.2%, and the total amount of all curcumin compounds in the turmeric extract is 96.5-97.3%.
Description
Technical Field
The invention belongs to the technical field of extraction, and particularly relates to a preparation method of turmeric extract.
Background
Turmeric is a dried rhizome of Curcuma longa L, a common traditional Chinese medicine in Chinese pharmacopoeia. The main functions of the medicine are blood breaking, qi moving, dysmenorrhea and pain relieving. Can be used for treating chest and hypochondrium pain, chest pain, dysmenorrhea, amenorrhea, abdominal mass, rheumatic shoulder and arm pain, and traumatic injury.
Turmeric is a common drug, and its main bioactive components are curcumin and volatile oil. The former has the effects of reducing blood lipid, anticoagulation, antioxidation, cholagogic, anticancer, etc.; the latter mainly plays an anti-inflammatory, antibacterial and cough relieving role. Curcumin exerts anticancer effect by inducing malignant tumor cell differentiation and tumor cell apoptosis and inhibiting effect on various stages of tumor growth, and has wide clinical application.
The method for extracting curcumin is various, for example, the method for extracting curcumin from turmeric by adopting an organic solvent (such as ethanol) is a technology commonly adopted at home and abroad at present. However, the turmeric extract extracted by the method is a mixture of curcumin, lipid and other impurities, the product has low pigment content, and the quality index that the total pigment content is more than or equal to 90 percent and is difficult to dry, which is required by FAO/WHO standard.
In order to solve the above problems, the patent document with the patent number 201710051021.X adopts an ethanol crystallization method to prepare the turmeric extract, and realizes the separation of turmeric compounds and turmeric oil substances in the crystallization step, thereby fundamentally solving the problem that the turmeric extract is difficult to dry. However, the patent document adopts petroleum ether for degreasing, and petroleum ether is a light petroleum product, is a mixture of hydrocarbons (mainly pentane and hexane) with low relative molecular weight, is easy to volatilize, and vapor and air of the petroleum ether can form an explosive mixture to cause combustion explosion when meeting open fire and high heat energy, so that great challenges are brought to the safety and environmental protection of operation; and two-step lower alcohol crystallization is required, increasing the complexity of the operation.
Disclosure of Invention
The invention mainly aims to provide a preparation method of turmeric extract, which does not need petroleum ether extraction degreasing and 2 times of ethanol crystallization, has simpler operation and obvious degreasing effect, is favorable for drying, and is safer and more environment-friendly in the whole extraction process.
A preparation method of turmeric extract comprises the following steps:
1) Drying Curcuma rhizome decoction pieces at 45-80deg.C for 24-72 hr;
2) Adding solvent into the turmeric decoction pieces obtained in the step 1) for extraction for 2-4 times, wherein the extraction time is 1-4 hours each time, and the extraction temperature is 45-80 ℃;
3) Concentrating the extract obtained in the step 2) to 0.1-1 times of the weight of turmeric decoction pieces, refrigerating at 2-8deg.C, standing for precipitation for 2-5 days, centrifuging, and collecting crystals;
4) Adding 80-95% lower alcohol solution into the crystals collected in the step 3), stirring uniformly, centrifuging, washing 2-4 times with 80-95% lower alcohol solution, and centrifuging to obtain crystals;
5) Drying the crystal obtained in the step 4) to obtain the turmeric extract.
Preferably, the step 1) is preceded by crushing and sieving the turmeric medicinal material to obtain turmeric decoction pieces.
Preferably, the solvent in the step 2) is a 50% -95% lower alcohol solution or a mixed solution of acetone and n-hexane.
Preferably, the lower alcohol is methanol, ethanol, propanol, butanol, pentanol or hexanol.
Preferably, the mass ratio of acetone to n-hexane is (1-2): (1-2).
Preferably, the addition amount of the extraction solvent is 6-20 times of the weight of turmeric decoction pieces.
Preferably, the crystals obtained in step 4) are dried below 60 ℃ until the moisture content is below 8%.
The beneficial effects of the invention are as follows:
1) According to the invention, the step of extracting and degreasing petroleum ether is omitted, but turmeric is baked before extraction, so that volatile oil in turmeric can be removed, the volatile oil removing effect is obvious, and the separation of curcumin compounds and volatile oil is realized, thereby being beneficial to drying turmeric extract; in addition, petroleum ether degreasing is not needed, so that the whole extraction process is safer and more environment-friendly;
2) Compared with the prior art, the method omits 2 times of ethanol crystallization steps, and directly crystallizes in the cold storage and standing stage, and the yield of the turmeric extract is not affected;
3) Test results show that by adopting the method provided by the invention, the curcumin content in the turmeric extract is between 55.4 and 57.3 percent, the curcumin compound content is between 66.3 and 69.1 percent, the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin is between 64.3 and 67.2 percent, and the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin in the turmeric extract is between 96.5 and 97.3 percent, so that the method accords with the feeding use characteristics of the lipid-lowering and vein-relaxing soft capsule.
Detailed Description
The invention provides a preparation method of turmeric extract, which comprises the following steps:
1) Drying Curcuma rhizome decoction pieces at 45-80deg.C for 24-72 hr;
2) Adding solvent into the turmeric decoction pieces obtained in the step 1) for extraction for 2-4 times, wherein the extraction time is 1-4 hours each time, and the extraction temperature is 45-80 ℃;
3) Concentrating the extract obtained in the step 2) to 0.1-1 times of the weight of turmeric decoction pieces, refrigerating at 2-8deg.C, standing for precipitation for 2-5 days, centrifuging, and collecting crystals;
4) Adding 80-95% lower alcohol solution into the crystals collected in the step 3), stirring uniformly, centrifuging, washing 2-4 times with 80-95% lower alcohol solution, and centrifuging to obtain crystals;
5) Drying the crystal obtained in the step 4) to obtain the turmeric extract.
According to the invention, the turmeric decoction pieces are baked before extraction, so that volatile oil in the turmeric decoction pieces can be removed, and the volatile oil removal effect is obvious. Compared with the prior art, the method omits 2 times of ethanol crystallization steps, directly crystallizes in a refrigerating and standing stage, the yield of the turmeric extract is not affected, the curcumin content in the turmeric extract is between 55.4 and 57.3 percent, the curcumin compound content is between 66.3 and 69.1 percent, the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin is between 64.3 and 67.2 percent, and the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin is between 96.5 and 97.3 percent in the turmeric extract, so that the method accords with the feeding use characteristics of the lipid-lowering and vein-relaxing soft capsule.
The soft capsule for reducing blood fat and dredging collaterals is characterized in that the curcumin in the turmeric extract is 40.0-60.0%, the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin is 45.0-70.0%, and the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin accounts for more than 93.0% of curcumin compounds in the turmeric extract.
In order to improve the baking effect and the volatile oil removing effect in the turmeric decoction pieces, the turmeric decoction pieces are crushed and sieved before the step 1). The invention is not limited to the sieve, and can be a No. 2 sieve.
The solvent in the step 2) is 50-95% lower alcohol solution or mixed solution of acetone and n-hexane. Wherein the addition amount of each extraction solvent is 6-20 times of the weight of Curcuma rhizome decoction pieces. Wherein when the solvent is a mixed solution of acetone and n-hexane, the mass ratio of the acetone to the n-hexane is (1-2): (1-2).
In addition, the crystals in step 5) are dried at a temperature below 60 ℃ until the moisture content is below 8%.
In the present invention, the lower alcohol mentioned is methanol, ethanol, propanol, butanol, pentanol or hexanol, preferably ethanol.
The sources of the lower alcohol, the acetone, the n-hexane and the turmeric medicinal materials are not limited, and the medicines are all commercially available.
In order to further illustrate the present invention, the following examples are provided.
Example 1
1) Pulverizing Curcuma rhizome 1kg into coarse powder, sieving with No. 2 sieve, and baking at 45deg.C for 72 hr to obtain Curcuma rhizome decoction pieces;
2) Putting the turmeric decoction pieces in the step 1) into an extraction tank, adding a mixture solution of acetone and n-hexane with the mass ratio of 1:2, wherein the mass of the mixture solution of acetone and n-hexane is 9 times that of the turmeric decoction pieces, stirring and extracting for 2 times, extracting for 3h and 2h respectively, extracting at 60 ℃ each time, collecting upper layer extracting solution after the extraction is finished, and merging the extracting solutions for 2 times;
3) Concentrating the extract obtained in the step 2) in vacuum to obtain paste which is 0.2 times of the weight of turmeric decoction pieces, refrigerating, standing and precipitating the paste at 2 ℃ for 3 days, centrifuging, and collecting crystals;
4) Adding 95% ethanol solution into the crystals after centrifugation in the step 3), stirring uniformly, centrifuging, and leaching for 2 times by using 95% ethanol to obtain crystals;
5) Drying the crystals obtained in the step 4) at 40 ℃ until the water content is below 8%, thus obtaining the turmeric extract.
Example 2
1) Pulverizing Curcuma rhizome 1kg into coarse powder, sieving with No. 2 sieve, and baking at 60deg.C for 48 hr to obtain Curcuma rhizome decoction pieces;
2) Putting the turmeric decoction pieces in the step 1) into an extraction tank, adding an ethanol solution with the mass concentration of 70%, wherein the mass of the ethanol solution is 9 times that of the turmeric decoction pieces, stirring and extracting for 2 times, wherein the extracting time is respectively 2.5 hours and 2 hours, the extracting temperature of each time is 60 ℃, collecting the upper layer extracting solution after the extracting is finished, and combining the extracting solutions for 2 times;
3) Concentrating the extract obtained in the step 2) in vacuum to obtain paste which is 0.2 times of the weight of decoction pieces, refrigerating, standing and precipitating the paste for 4 days at 8 ℃, centrifuging, and collecting crystals;
4) Adding ethanol with the mass concentration of 90% into the crystals collected in the step 3), uniformly stirring, centrifuging, and leaching for 3 times by adding ethanol with the mass concentration of 90% to obtain crystals;
5) Drying the crystals obtained in the step 4) at 60 ℃ until the water content is below 8%, thus obtaining the turmeric extract.
Example 3
1) Pulverizing Curcuma rhizome 1kg into coarse powder, sieving with No. 2 sieve, and baking at 80deg.C for 24 hr to obtain Curcuma rhizome decoction pieces;
2) Putting the turmeric decoction pieces in the step 1) into an extraction tank, adding a mixture solution of acetone and n-hexane with the mass ratio of 1:2, wherein the mass of the mixture solution of acetone and n-hexane is 9 times that of the turmeric decoction pieces, stirring and extracting for 2 times, extracting for 2h and 1.5h respectively, extracting at 55 ℃ each time, collecting the upper layer extract after the extraction is finished, and combining the 2 times of extract;
3) Concentrating the extract obtained in the step 2) in vacuum to obtain paste which is 0.18 times of the weight of decoction pieces, refrigerating, standing and precipitating at 5 ℃ for 5 days, centrifuging, and collecting crystals;
4) Adding 80% ethanol into the crystals collected in the step 3), stirring uniformly, centrifuging, and leaching for 4 times by adding 80% ethanol to obtain crystals;
5) Drying the crystal obtained in the step 4) at 40 ℃ until the water content is below 8%, and pulverizing to obtain the turmeric extract.
Example 4
1) Pulverizing Curcuma rhizome 1kg into coarse powder, sieving with No. 2 sieve, and baking at 50deg.C for 72 hr to obtain Curcuma rhizome decoction pieces;
2) Putting the turmeric decoction pieces in the step 1) into an extraction tank, adding an ethanol solution with the mass concentration of 50%, wherein the addition amount of the ethanol solution is 10 times of the turmeric decoction pieces, stirring and extracting for 2 times, wherein the extracting time is respectively 2 hours and 1.5 hours, the extracting temperature of each time is 55 ℃, collecting the upper layer extracting solution after the extracting is finished, and combining the extracting solutions for 2 times;
3) Concentrating the extract obtained in the step 2) in vacuum to obtain paste which is 0.1 time of the weight of decoction pieces, refrigerating, standing and precipitating at 6 ℃ for 3 days, centrifuging, and collecting precipitate;
4) Adding 80% ethanol into the crystals collected in the step 3), stirring uniformly, centrifuging, and leaching for 3 times by adding 80% ethanol to obtain crystals;
5) Drying the crystal obtained in the step 4) at 30 ℃ until the water content is below 8%, and pulverizing to obtain the turmeric extract.
Example 5
1) Pulverizing Curcuma rhizome 1kg into coarse powder, sieving with No. 2 sieve, and baking at 70deg.C for 24 hr to obtain Curcuma rhizome decoction pieces;
2) Putting the turmeric decoction pieces in the step 1) into an extraction tank, adding a mixture solution of acetone and n-hexane with the mass ratio of 1:1, wherein the addition amount of the mixture solution of acetone and n-hexane is 8 times that of the turmeric decoction pieces, stirring and extracting for 2 times at 65 ℃ respectively for 2 hours and 2 hours, collecting upper-layer extracting solutions after the extraction is finished, mixing 2 times of filtrate, and filtering to obtain filtrate;
3) Concentrating the extract obtained in the step 2) in vacuum to obtain paste which is 0.16 times of the weight of decoction pieces, refrigerating, standing and precipitating the paste for 4 days at 5 ℃, centrifuging, and collecting crystals;
4) Adding ethanol with the mass concentration of 85% into the crystals collected in the step 3), uniformly stirring, centrifuging, and leaching for 4 times by adding ethanol with the mass concentration of 85% to obtain crystals;
5) Drying the crystal obtained in the step 4) at 30 ℃ until the water content is below 8%, and pulverizing to obtain the turmeric extract.
Comparative example 1
Based on example 4, comparative example 1 differs from example 4 only in that the baking temperature in step 1) is 40℃and the remainder is the same as example 4.
Comparative example 2
Based on example 5, comparative example 1 differs from example 5 only in that the baking temperature in step 1) is 90℃and the remainder is the same as example 5.
Comparative example 3
Based on example 5, the difference between comparative example 1 and example 5 is that 1kg of turmeric material is taken in step 1), pulverized into coarse powder, and sieved through a No. 2 sieve to obtain turmeric decoction pieces, and the rest is the same as example 5.
The volatile oil in turmeric decoction pieces obtained in examples 1 to 5 and comparative examples 1 to 3 was measured according to the volatile oil measurement method of chinese pharmacopoeia 2015, and the results are shown in table 1.
TABLE 1 detection results
| Volatile oil content/% | |
| Example 1 | 0.7 |
| Example 2 | 0.8 |
| Example 3 | 0.6 |
| Example 4 | 0.7 |
| Example 5 | 0.7 |
| Comparative example 1 | 5.3 |
| Comparative example 2 | 0.6 |
| Comparative example 3 | 7.2 |
As can be seen from table 1, turmeric is baked at 45-80 ℃ to effectively remove volatile oil from turmeric; when the baking temperature is less than 45 ℃, the volatile oil in the turmeric is not easy to remove; when the baking temperature is higher than 80 ℃, the excessive volatile oil is not removed from the turmeric.
The quality of the turmeric extracts obtained in examples 1 to 5 and comparative examples 1 to 3, and the content of curcumin compounds, curcumin, demethoxycurcumin, bisdemethoxycurcumin in turmeric extract were measured, and the results are shown in Table 2.
The quality of the turmeric extract and the content of curcumin compounds, curcumin, demethoxycurcumin and bisdemethoxycurcumin in the turmeric extract are detected according to the quality standard of the lipid-lowering and vein-relaxing soft capsule of the 2020 edition of Chinese pharmacopoeia.
Wherein the content of curcuminoids = mass of curcuminoids/mass of curcuminoids extract x 100%;
curcumin content = curcumin mass/turmeric extract mass x 100%;
demethoxycurcumin content = demethoxycurcumin mass/turmeric extract mass x 100%;
content of bisdemethoxycurcumin = mass of bisdemethoxycurcumin/mass of turmeric extract x 100%.
Table 2 measurement results
As can be seen from Table 2, in examples 1-5, the curcumin content was between 55.4 and 57.3%, the curcumin content was between 66.3 and 69.1%, the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin was between 64.3 and 67.2%, and the total amount of curcumin, demethoxycurcumin and bisdemethoxycurcumin was between 96.5 and 97.3% of the total amount of all curcumin compounds in the turmeric extract; the curcumin extract obtained by extraction in the examples 1-5 accords with the feeding characteristics of the soft capsule for reducing blood fat and dredging collaterals.
In comparative examples 1 to 3, the total amount of moisture and curcumin, demethoxycurcumin, bisdemethoxycurcumin of comparative example 1 did not meet the quality standard; the proportion of the total amount of curcumin, demethoxycurcumin, bisdemethoxycurcumin, curcumin compounds, curcumin, demethoxycurcumin and bisdemethoxycurcumin in the curcumin compounds in comparative example 2 does not meet the quality standard, and the comparative example 3 does not precipitate crystals and does not meet the feeding use characteristics of the lipid-lowering and vein relaxing soft capsules.
The foregoing description is only of the preferred embodiments of the invention, and it is apparent that the embodiments described are merely some, but not all, of the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (3)
1. A method for preparing turmeric extract, comprising the steps of:
1) Drying Curcuma rhizome decoction pieces at 45-80deg.C for 24-72 hr;
2) Adding solvent into the turmeric decoction pieces obtained in the step 1) for extraction for 2-4 times, wherein the extraction time is 1-4 hours each time, and the extraction temperature is 45-80 ℃;
3) Concentrating the extract obtained in the step 2) to 0.1-1 times of the weight of turmeric decoction pieces, refrigerating at 2-8deg.C, standing for precipitation for 2-5 days, centrifuging, and collecting crystals;
4) Adding 80-95% lower alcohol solution into the crystals collected in the step 3), stirring uniformly, centrifuging, and washing 2-4 times with 80-95% lower alcohol solution to obtain crystals;
5) Drying the crystals obtained in the step 4) to obtain turmeric extract;
the step 1) is preceded by crushing and sieving turmeric medicinal materials to obtain turmeric decoction pieces;
the solvent in the step 2) is 50% -95% lower alcohol solution or mixed solution of acetone and n-hexane;
the addition amount of each extraction solvent is 6-20 times of the weight of turmeric decoction pieces;
drying the crystals obtained in the step 4) below 60 ℃ until the moisture content is below 8%.
2. The method for preparing turmeric extract as claimed in claim 1, wherein the lower alcohol is methanol, ethanol, propanol, butanol, pentanol or hexanol.
3. The method for preparing turmeric extract according to claim 1, wherein the mass ratio of acetone to n-hexane is (1-2): (1-2).
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| CN202210985968.9A CN115403457B (en) | 2022-08-16 | 2022-08-16 | A method for preparing Curcuma rhizome extract |
| PCT/CN2023/094272 WO2024037071A1 (en) | 2022-08-16 | 2023-05-15 | Method for preparing curcuma extract |
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| CN102603505A (en) * | 2012-02-09 | 2012-07-25 | 徐宏永 | Method for extracting and separating high-purity curcumin with low heavy-metal residues from turmeric |
| CN102617316B (en) * | 2012-03-13 | 2013-10-30 | 宁波中药制药有限公司 | Method for extracting curcumin from turmeric |
| CN103071117B (en) * | 2013-01-18 | 2014-01-08 | 四川汇丰生物科技有限公司 | Method for extracting curcuma oil and curcumine from rhizoma curcumae longae |
| CN103463567B (en) * | 2013-02-28 | 2015-07-15 | 成都中医药大学 | Vinegar rhizoma curcumae decoction piece and processing method thereof |
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| CN108339086A (en) * | 2017-01-23 | 2018-07-31 | 神威药业集团有限公司 | A kind of preparation method of Turmeric P.E |
| CN110771892B (en) * | 2019-11-12 | 2023-05-16 | 晨光生物科技集团股份有限公司 | High-quality curcumin product, production method and application thereof |
| CN110724045B (en) * | 2019-11-12 | 2022-06-21 | 晨光生物科技集团股份有限公司 | Preparation method of curcumin with low solvent residue |
| CN112535717A (en) * | 2020-12-08 | 2021-03-23 | 宁波杰顺生物科技有限公司 | Turmeric extract and preparation method thereof |
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