CN107805193A - The production method of low molten residual turmeric cellulose crystal - Google Patents
The production method of low molten residual turmeric cellulose crystal Download PDFInfo
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- CN107805193A CN107805193A CN201711205171.8A CN201711205171A CN107805193A CN 107805193 A CN107805193 A CN 107805193A CN 201711205171 A CN201711205171 A CN 201711205171A CN 107805193 A CN107805193 A CN 107805193A
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Abstract
The present invention relates to a kind of production method of low molten residual turmeric cellulose crystal, belong to natural extract technical field.Comprise the following steps：（1）Add propane diols into turmeric paste, desolvation is to total solvent residual quantity≤10ppm after heating, stirring；（2）Refining agent is added, after heating, stirring, pure water is added, is centrifuged after continuing stirring, described refining agent is mass ratio 1:0.5~1 Tween 80 and the mixture of propane diols；（3）Hot water is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again, gained lower sediment thing is turmeric cellulose crystal crude product；（4）By the vacuum drying of turmeric cellulose crystal crude product, crush, obtain low molten residual turmeric cellulose crystal.Gained curcumin crystal purity of the invention is higher than 95%, and content yield is higher than 40%, and total solvent residual quantity is less than 10ppm, and product has security, trophism and feature concurrently；And technique is simple, it is easy to industrialized production.
Description
Technical field
The invention belongs to natural extract technical field, and in particular to a kind of production method of low molten residual turmeric cellulose crystal.
Background technology
Turmeric is Zingiber（Zingiberaceae）Turmeric（Curcuma Linn. ）Plant turmeric（Curcuma longa
L.）Dry rhizome, the plantation of turmeric can be traced back to away from before modern more than 6,000 years, on China, India and Southeast Asia and other places
Distribution.The traditional Chinese medical science thinks that turmeric medicinal plant has promoting the circulation of qi blood-breaking, Xiao Ji Zhi Tong, heart fire-clearing upset-relieving and other effects, main in turmeric
Active ingredient is curcumin chemical compounds, with curcumin (curcumin, Cur), Demethoxycurcumin
(demethoxycurcumin, DMC), Bisdemethoxycurcumin (bisdemethoxycurcumin, BDMC) are most commonly seen,
Curcumin chemical compounds are referred to as " curcumin ".
At present, the large-scale production of turmeric cellulose crystal is broadly divided into two steps, and the first step is extraction, former from turmeric first
Extraction obtains turmeric crude extract, referred to as turmeric paste in material；Second step is refined, using turmeric paste as raw material, is refining to obtain ginger
Flavine crystal.Industrial common turmeric paste extraction and curcumin refine and use organic solvent extraction, but due to ginger
Flavine molecule has two kinds of dynamic isomers of keto-acid and enol form, intramolecular or the easy formation hydrogen bond between solvent molecule, conventional
Solvent removal method can not thoroughly remove organic solvent in turmeric paste and turmeric cellulose crystal, cause turmeric paste and turmeric
Organic solvent residual height in cellulose crystal is higher, the total solvent residual in the turmeric paste and turmeric cellulose crystal in China market
Amount directly affects normal use of the curcumin product as food additives in more than 1000ppm.
The content of the invention
The shortcomings that in order to overcome prior art, the present invention provide a kind of production method of low molten residual turmeric cellulose crystal, we
Method is simple to operate, is easy to industrialized production, and products obtained therefrom solvent residual amount is low.To solve above technical problem, the present invention is adopted
Technical scheme is as follows：
A kind of production method of low molten residual turmeric cellulose crystal, comprises the following steps：
（1）Add propane diols into turmeric paste, desolvation is to total solvent residual quantity≤10ppm after heating, stirring；
（2）Refining agent is added, after heating, stirring, pure water is added, is centrifuged after continuing stirring, described refining agent is quality
Than 1:0.5~1 Tween-80 and the mixture of propane diols；
（3）Hot water is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again, gained lower sediment thing
As turmeric cellulose crystal crude product；
（4）By the vacuum drying of turmeric cellulose crystal crude product, crush, obtain low molten residual turmeric cellulose crystal.
Step of the present invention（1）Turmeric cellulose content in middle turmeric paste is 20~30%；The propane diols is 1,2- third
Glycol or 1,3-PD, its quality are 0.2~0.5 times of turmeric paste quality.
Step of the present invention（1）Middle heating-up temperature is 40~50 DEG C, and mixing time is 1~2h.
Step of the present invention（1）Vacuum >=0.08MPa of middle desolvation, temperature be 50~80 DEG C, the time be 1~
3h。
Step of the present invention（2）The mass ratio of middle refining agent and turmeric paste is 1~2:1, heated after adding refining agent
Temperature is 60~70 DEG C, and mixing time is 0.5~1h；The propane diols is 1,2- propane diols or 1,3- propane diols.
Step of the present invention（2）The quality of middle pure water is 10~20 times of turmeric paste quality.
Step of the present invention（2）It is middle add pure water concrete operation step be：Treat the mixing of turmeric paste and refining agent
Thing is cooled to 50~55 DEG C, under agitation, is slowly added to 4~6 times pure water consistent with mixture temperature, and stirring 30~
60min, treat that slow cooling to 30~35 DEG C, adds remaining pure water, continues 4~5h of stirring.
Step of the present invention（3）The temperature of hot water is 90~100 DEG C, and the mass ratio of hot water and turmeric paste is 1:1.
Step of the present invention（2）、（3）Middle centrifugal condition is centrifugal rotational speed >=4000r/m, centrifugation time >=2min.
Step of the present invention（4）Vacuum drying condition is 0.08~0.095MPa of vacuum, 80~100 DEG C of temperature.
The beneficial effects of the present invention are：Gained curcumin crystal purity of the invention is higher than 95%, and content yield is higher than 40%,
Total solvent residual quantity is less than 10ppm, substantially increases edible safety of the turmeric cellulose crystal as food additives, makes product simultaneous
There are security, trophism and feature；Present invention process is simple, is easy to industrialized production.
Embodiment
Embodiment 1
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 20.0%, total organic solvent residual quantity 1100ppm.Xiang Qi
Middle addition 10.0g1,2- propane diols, after being heated under the conditions of 40 DEG C and stirring 2h, solvent removed by vacuum, vacuum 0.08MPa,
Temperature 50 C, time 3h, it is 10ppm to detect its total solvent residual quantity.
（2）Add 70g mass ratioes 1:0.5 Tween-80 and the mixture of 1,2-PD, are heated under the conditions of 60 DEG C
And after stirring 30min, slow cooling, when objects system temperature to be mixed is down to 55 DEG C, under agitation, it is slowly added to 250.0g
Temperature is 55 DEG C of pure water, stirs 30min, then slow cooling to 35 DEG C, continuously adds 250.0g pure water, is centrifuged after stirring 5h, from
The heart rotating speed 5000r/m, centrifugation time 2min.
（3）It is 90 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.08MPa, 100 DEG C, crush, obtain low molten residual
Turmeric cellulose crystal 4.3g.
After testing, turmeric cellulose crystal total solvent residual quantity 8ppm, content 95.1%, total content yield 40.9%.
Embodiment 2
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 30.0%, total organic solvent residual quantity 1500ppm.Xiang Qi
Middle addition 25.0g1, ammediol, after being heated under the conditions of 50 DEG C and stirring 110min, solvent removed by vacuum, vacuum
0.095MPa, 80 DEG C, time 1h of temperature, it is 8ppm to detect its total solvent residual quantity.
（2）Add 100g mass ratioes 1:1 Tween-80 and the mixture of 1,3-PD, are heated simultaneously under the conditions of 70 DEG C
After stirring 1h, slow cooling, when objects system temperature to be mixed is down to 50 DEG C, under agitation, 230.0g temperature is slowly added to
For 50 DEG C of pure water, 30min, then slow cooling are stirred to 30 DEG C, continuously adds 750.0g pure water, is centrifuged after stirring 4h, centrifugation turns
Fast 4000r/m, centrifugation time 2min.
（3）It is 100 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.095MPa, 80 DEG C, crush, obtain low molten residual
Turmeric cellulose crystal 6.5g.
After testing, turmeric cellulose crystal total solvent residual quantity 8ppm, content 95.2%, total content yield 41.3%.
Embodiment 3
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 24.8%, total organic solvent residual quantity 1055ppm.Xiang Qi
Middle addition 15.0g1,2- propane diols, after being heated under the conditions of 45 DEG C and stirring 1.5h, solvent removed by vacuum, vacuum
0.085MPa, temperature 70 C, time 2h, it is 9ppm to detect its total solvent residual quantity.
（2）Add 75g mass ratioes 1:0.7 Tween-80 and the mixture of 1,3-PD, are heated under the conditions of 65 DEG C
And after stirring 45min, slow cooling, when objects system temperature to be mixed is down to 52 DEG C, under agitation, it is slowly added to 250.0g
Temperature is 52 DEG C of pure water, stirs 45min, then slow cooling to 33 DEG C, continuously adds 600.0g pure water, is centrifuged after stirring 4.5h,
Centrifugal rotational speed 4000r/m, centrifugation time 5min.
（3）It is 95 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.09MPa, 90 DEG C, crush, obtain low molten residual ginger
Flavine crystal 5.5g.
After testing, turmeric cellulose crystal total solvent residual quantity 7ppm, content 95.5%, total content yield 42.4%.
Embodiment 4
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 25.2%, total organic solvent residual quantity 1050ppm.Xiang Qi
Middle addition 20.0g1, ammediol, after being heated under the conditions of 50 DEG C and stirring 1h, solvent removed by vacuum, vacuum 0.085MPa,
Temperature 60 C, time 2h, it is 10ppm to detect its total solvent residual quantity.
（2）Add 50.0g mass ratioes 1:0.5 Tween-80 and the mixture of 1,2-PD, add under the conditions of 60 DEG C
Heat and after stirring 30min, slow cooling, when objects system temperature to be mixed is down to 50 DEG C, under agitation, is slowly added to
250.0g temperature is 50 DEG C of pure water, stirs 30min, then slow cooling is to 30 DEG C, continuously adds 450.0g pure water, stir after 4h from
The heart, centrifugal rotational speed 4000r/m, centrifugation time 3min.
（3）It is 90 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.09MPa, 85 DEG C, crush, obtain low molten residual ginger
Flavine crystal 5.7g.
After testing, turmeric cellulose crystal total solvent residual quantity 9ppm, content 95.4%, total content yield 43.2%.
Embodiment 5
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 28.3%, total organic solvent residual quantity 2000ppm.Xiang Qi
Middle addition 20.0g1,2- propane diols, after being heated under the conditions of 48 DEG C and stirring 2h, solvent removed by vacuum, vacuum 0.095MPa,
Temperature 50 C, time 1h, it is 9ppm to detect its total solvent residual quantity.
（2）Add 60.0g mass ratioes 1:0.8 Tween-80 and the mixture of 1,2-PD, add under the conditions of 70 DEG C
Heat and after stirring 50min, slow cooling, when objects system temperature to be mixed is down to 54 DEG C, under agitation, is slowly added to
280.0g temperature is 54 DEG C of pure water, stirs 50min, then slow cooling is to 31 DEG C, continuously adds 650.0g pure water, stir after 4h from
The heart, centrifugal rotational speed 4200r/m, centrifugation time 3min.
（3）It is 98 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.092MPa, 95 DEG C, crush, obtain low molten residual
Turmeric cellulose crystal 6.2g.
After testing, turmeric cellulose crystal total solvent residual quantity 8ppm, content 95.1%, total content yield 41.7%.
Embodiment 6
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 21.7%, total organic solvent residual quantity 1269ppm.Xiang Qi
Middle addition 16.0g1,2- propane diols, after being heated under the conditions of 47 DEG C and stirring 70min, solvent removed by vacuum, vacuum
0.08MPa, 58 DEG C, time 80min of temperature, it is 9ppm to detect its total solvent residual quantity.
（2）Add 55g mass ratioes 1:0.9 Tween-80 and the mixture of 1,2-PD, are heated under the conditions of 62 DEG C
And after stirring 35min, slow cooling, when objects system temperature to be mixed is down to 55 DEG C, under agitation, it is slowly added to 200.0g
Temperature is 55 DEG C of pure water, stirs 30min, then slow cooling is to 34 DEG C, continuously adds 800.0g pure water, stir after 250min from
The heart, centrifugal rotational speed 4500r/m, centrifugation time 2min.
（3）It is 92 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.95MPa, 98 DEG C, crush, obtain low molten residual ginger
Flavine crystal 4.9g.
After testing, turmeric cellulose crystal total solvent residual quantity 7ppm, content 96.4%, total content yield 43.5%.
Embodiment 7
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 27.5%, total organic solvent residual quantity 1885ppm.Xiang Qi
Middle addition 24.0g1, ammediol, after being heated under the conditions of 44 DEG C and stirring 100min, solvent removed by vacuum, vacuum
0.095MPa, 75 DEG C, time 2.5h of temperature, it is 10ppm to detect its total solvent residual quantity.
（2）Add 90g mass ratioes 1:0.9 Tween-80 and the mixture of 1,3-PD, are heated under the conditions of 68 DEG C
And after stirring 60min, slow cooling, when objects system temperature to be mixed is down to 51 DEG C, under agitation, it is slowly added to 250.0g
Temperature is 51 DEG C of pure water, stirs 60min, then slow cooling is to 35 DEG C, continuously adds 300.0g pure water, stir after 290min from
The heart, centrifugal rotational speed 4800r/m, centrifugation time 3min.
（3）It is 96 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.087MPa, 90 DEG C, crush, obtain low molten residual
Turmeric cellulose crystal 6.0g.
After testing, turmeric cellulose crystal total solvent residual quantity 10ppm, content 97.2%, total content yield 42.4%.
Embodiment 8
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 23.4%, total organic solvent residual quantity 1712ppm.Xiang Qi
Middle addition 18.0g1,2- propane diols, after being heated under the conditions of 47 DEG C and stirring 80min, solvent removed by vacuum, vacuum
0.09MPa, 65 DEG C, time 170min of temperature, it is 10ppm to detect its total solvent residual quantity.
（2）Add 100g mass ratioes 1:0.6 Tween-80 and the mixture of 1,3-PD, are heated under the conditions of 64 DEG C
And after stirring 40min, slow cooling, when objects system temperature to be mixed is down to 53 DEG C, under agitation, it is slowly added to 300.0g
Temperature is 53 DEG C of pure water, stirs 30min, then slow cooling is to 32 DEG C, continuously adds 700.0g pure water, stir after 280min from
The heart, centrifugal rotational speed 6000r/m, centrifugation time 2min.
（3）It is 95 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.085MPa, 80 DEG C, crush, obtain low molten residual
Turmeric cellulose crystal 5.4g.
After testing, turmeric cellulose crystal total solvent residual quantity 8ppm, content 96.6%, total content yield 44.6%.
Embodiment 9
（1）Turmeric paste 50.0g is taken, after testing, its turmeric cellulose content 29.1%, total organic solvent residual quantity 2026ppm.Xiang Qi
Middle addition 22.0g1, ammediol, after being heated under the conditions of 49 DEG C and stirring 90min, solvent removed by vacuum, vacuum
0.088MPa, 80 DEG C, time 100min of temperature, it is 9ppm to detect its total solvent residual quantity.
（2）Add 80g mass ratioes 1:1 Tween-80 and the mixture of 1,2-PD, are heated simultaneously under the conditions of 66 DEG C
After stirring 55min, slow cooling, when objects system temperature to be mixed is down to 52 DEG C, under agitation, 200.0g temperature is slowly added to
Spend and continuously add 300.0g pure water to 33 DEG C for 52 DEG C of pure water, stirring 40min, then slow cooling, centrifuge, centrifuge after stirring 5h
Rotating speed 4000r/m, centrifugation time 2min.
（3）It is 100 DEG C of hot water that 50.0g temperature is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again
Separation, centrifugal rotational speed 4000r/m, centrifugation time 2min, gained lower sediment thing are turmeric cellulose crystal crude product.
（4）After turmeric cellulose crystal crude product is dried under the conditions of vacuum 0.08MPa, 82 DEG C, crush, obtain low molten residual ginger
Flavine crystal 6.6g.
After testing, turmeric cellulose crystal total solvent residual quantity 7ppm, content 95.9%, total content yield 43.5%.
Claims (10)
1. a kind of production method of low molten residual turmeric cellulose crystal, it is characterised in that comprise the following steps：
（1）Add propane diols into turmeric paste, desolvation is to total solvent residual quantity≤10ppm after heating, stirring；
（2）Refining agent is added, after heating, stirring, pure water is added, is centrifuged after continuing stirring, described refining agent is quality
Than 1:0.5~1 Tween-80 and the mixture of propane diols；
（3）Hot water is added into the lower sediment thing after centrifugation, after stirring, is centrifuged again, gained lower sediment thing
As turmeric cellulose crystal crude product；
（4）By the vacuum drying of turmeric cellulose crystal crude product, crush, obtain low molten residual turmeric cellulose crystal.
2. the production method of low molten residual turmeric cellulose crystal according to claim 1, it is characterised in that the step（1）In
Turmeric cellulose content in turmeric paste is 20~30%；The propane diols is 1,2-PD or 1,3-PD, and its quality is ginger
0.2~0.5 times of yellow medicinal extract quality.
3. the production method of low molten residual turmeric cellulose crystal according to claim 1, it is characterised in that the step（1）In
Heating-up temperature is 40~50 DEG C, and mixing time is 1~2h.
4. the production method of low molten residual turmeric cellulose crystal according to claim 2, it is characterised in that the step（1）In
Vacuum >=0.08MPa of desolvation, temperature are 50~80 DEG C, and the time is 1~3h.
5. the production method of low molten residual turmeric cellulose crystal according to claim 1, it is characterised in that the step（2）In
The mass ratio of refining agent and turmeric paste is 1~2:1, heating-up temperature is 60~70 DEG C after adding refining agent, mixing time 0.5
~1h；The propane diols is 1,2- propane diols or 1,3- propane diols.
6. the production method of low molten residual turmeric cellulose crystal according to claim 1, it is characterised in that the step（2）In
The quality of pure water is 10~20 times of turmeric paste quality.
7. the production method of low molten residual turmeric cellulose crystal according to claim 6, it is characterised in that the step（2）In
Add pure water concrete operation step be：Treat that the mixture of turmeric paste and refining agent is cooled to 50~55 DEG C, in stirring condition
Under, 4~6 times pure water consistent with mixture temperature are slowly added to, 30~60min is stirred, treats slow cooling to 30~35 DEG C, then
Remaining pure water is added, continues 4~5h of stirring.
8. the production method of the low molten residual turmeric cellulose crystal according to claim 1-7 any one, it is characterised in that described
Step（3）The temperature of hot water is 90~100 DEG C, and the mass ratio of hot water and turmeric paste is 1:1.
9. the production method of the low molten residual turmeric cellulose crystal according to claim 1-7 any one, it is characterised in that described
Step（2）、（3）Middle centrifugal condition is centrifugal rotational speed >=4000r/m, centrifugation time >=2min.
10. the production method of the low molten residual turmeric cellulose crystal according to claim 1-7 any one, it is characterised in that institute
State step（4）Vacuum drying condition is 0.08~0.095MPa of vacuum, 80~100 DEG C of temperature.
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| CN112898359A (en) * | 2019-12-03 | 2021-06-04 | 晨光生物科技集团股份有限公司 | Preparation method of low-solubility residual crystal |
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| CN110724045A (en) * | 2019-11-12 | 2020-01-24 | 晨光生物科技集团股份有限公司 | Preparation method of curcumin with low solvent residue |
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| CN112898359A (en) * | 2019-12-03 | 2021-06-04 | 晨光生物科技集团股份有限公司 | Preparation method of low-solubility residual crystal |
| RU2759545C1 (en) * | 2020-12-07 | 2021-11-15 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method for dividing the sum of curcuminoids |
| CN113501750A (en) * | 2021-06-07 | 2021-10-15 | 哈工大机器人南昌智能制造研究院 | Method for continuously extracting curcuma oil and curcumin |
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