CN105754371A - Method for ultrasonic-assisted extraction of Caulis spatholobi pigment - Google Patents
Method for ultrasonic-assisted extraction of Caulis spatholobi pigment Download PDFInfo
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- CN105754371A CN105754371A CN201510455769.7A CN201510455769A CN105754371A CN 105754371 A CN105754371 A CN 105754371A CN 201510455769 A CN201510455769 A CN 201510455769A CN 105754371 A CN105754371 A CN 105754371A
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Abstract
The invention discloses a method for ultrasonic-assisted extraction of Caulis spatholobi pigment.The method includes: slicing, drying and smashing Caulis spatholobi to obtain Caulis spatholobi powder; using alcohol as extract, and performing ultrasonic extraction after sufficient stirring.The method has the advantages of high extraction efficiency, solvent saving, simple operation and convenience in extraction, extraction rate is up to 97.7%, and extraction takes 50 minutes only.
Description
Technical field
The invention belongs to biological field, be specifically related to a kind of method that ultrasonic assistant extracts Caulis Spatholobi pigment.
Background technology
Natural pigment is the food coloring obtained by natural resources.From microorganism (cultivation) and animal vegetable tissue, currently mainly obtain pigment, but major part is acquisition pigment from plant.Natural pigment not only has to the effect of food color, and major part natural pigment has physiologically active.Natural pigment has important effect in the application of food, health product, cosmetics and medicine all the time, the advantage such as is primarily due to it and has safety height, have no side effect.Existing 65 kinds of pigments in China's food service industry go through to use, including 48 kind of plant class pigments.Having 90% in the natural pigment that China produces every year for food colour, wherein, 20% natural pigment is extracted from plant and is obtained by fermentable, and all the other are caramel color.Abroad, the developed country such as especially American-European develops the new natural pigment of many kinds in food-processing industry.Natural pigment is increasingly paid attention to, and market is in continuous expansion.
Caulis Spatholobi is the dry rattan of leguminous plant spatholobus suberectus (Spatholobussuberectrus), have another name called Caulis Sargentodoxae, Sanguis sus domestica rattan, blood maple rattan, be distributed mainly on the ground such as Guangdong, Guangxi, Hainan, Jiangxi, Sichuan, Fujian, Yunnan, have enrich blood, invigorate blood circulation, the function of relaxing muscles and tendons and activating QI and blood in the collateral.Leukocyte, platelet and erythrocyte whole blood that the conventional Caulis Spatholobi disease that is alone or that be main prescription therapeutic such as chemicotherapy, blood system with Caulis Spatholobi of modern clinic causes reduce disease mutually.
Containing flavone in Caulis Spatholobi, the Multiple components such as triterpene and sterol, for non-anthocyanin class pigment, pigment content is high, there is good heat stability, non-oxidizability, reproducibility is all stronger, food additive and metal ion are little on the impact of its pigment, have to the effect of food color, it is a kind of safety, have no side effect and have nutrition and the natural food colour of medical value health care concurrently, therefore, from Caulis Spatholobi, extract a kind of rufous natural pigment and be applied to food additive, for increasing food colour kind, the development tool promoting China's food additive is of great significance.
At home and abroad, existing many scientific researchers research nature strength technique, and in major part extraction plant pigment technique, commonly used ultrasonic assistant method and extracted, and effect is better than traditional extracting technology.As Li great Jing et al. ultrasonic assistant method extracts the research of Testa sojae atricolor pigment, result shows that the pigment extraction ratio of ultrasonic assistant extraction process exceeds 8.3% than traditional water bath heating extraction, and the extraction rate reached of pigment is to 95.6%.Wang Jinting et al. ultrasonic method extracts Bauhinia aurea Levl research, it has been found that ultrasonic technique has advantages such as saving time, efficient, energy-conservation, and compared with Conventional solvents extraction, extraction time is foreshortened to 15min by 24h, compares solvent load with microwave method and decreases half.But ultrasonic assistant method is extracted Caulis Spatholobi red pigment and is had no domestic and international Research Literature report.
Summary of the invention
An object of the present invention is rare for solving natural additive source, that synthetic additive toxic and side effects is big problem, it is provided that a kind of ultrasonic assistant extracts the method for Caulis Spatholobi pigment.
The present invention provides a kind of method that ultrasonic assistant extracts Caulis Spatholobi pigment, and technical scheme is as follows: takes Caulis Spatholobi section, crushed after being dried, obtains Caulis Spatholobi powder；With ethanol for extracting solution, after being sufficiently stirred for, supersound extraction.
Further, described Caulis Spatholobi powder size is 100 orders.
Further, in described ethanol extract, concentration of alcohol is 40～80%, it is preferable that 60%.
Further, described ethanol extract pH=1～4, it is preferable that pH=2.
Further, described supersound extraction temperature is 40～80 DEG C, it is preferable that 70 DEG C.
Further, the described supersound extraction time is 30～50min, it is preferable that 30min.
Further, described Caulis Spatholobi powder and ethanol extract solid-liquid ratio are 1:30～1:50, it is preferable that 1:40.
Further, take Caulis Spatholobi section, crushed after being dried, obtain Caulis Spatholobi powder；With the solid-liquid ratio of 1:30, adding the ethanol extract of pH=2 in described Caulis Spatholobi powder, in described ethanol extract, concentration of alcohol is 50%；After being sufficiently stirred for, 70 DEG C of supersound extraction 50min.
Further, described supersound extraction number of times is 3 times.
The beneficial effects of the present invention is: the ultrasonic assistant of the present invention extracts the method for Caulis Spatholobi pigment, extracting solution pH, concentration of alcohol are investigated, Caulis Spatholobi pigment is extracted the impact of result by solid-liquid ratio, ultrasonic temperature, ultrasonic time and extraction time, pass through orthogonal test, obtain ultrasonic assistant and extract the best approach of Caulis Spatholobi pigment, the method compares with tradition leach extraction method, extraction efficiency is high, extraction time 50min is better than the time 90min needed for tradition extraction, save solvent, simple to operate, it is convenient to extract.
Accompanying drawing explanation
Fig. 1 show ultrasonic assistant of the present invention and extracts embodiment of the method 2 concentration of alcohol of Caulis Spatholobi pigment pigment extraction effect is affected figure；
Fig. 2 show ultrasonic assistant of the present invention and extracts the embodiment of the method 3pH of Caulis Spatholobi pigment pigment extraction effect is affected figure；
Fig. 3 show ultrasonic assistant of the present invention and extracts embodiment of the method 4 solid-liquid ratio of Caulis Spatholobi pigment pigment extraction effect is affected figure；
Fig. 4 show ultrasonic assistant of the present invention and extracts embodiment of the method 5 ultrasonic treatment time of Caulis Spatholobi pigment pigment extraction effect is affected figure；
Fig. 5 show ultrasonic assistant of the present invention and extracts embodiment of the method 6 temperature of Caulis Spatholobi pigment pigment extraction effect is affected figure；
Fig. 6 show ultrasonic assistant of the present invention and extracts embodiment of the method 9 extraction time of Caulis Spatholobi pigment pigment extraction effect is affected figure.
Detailed description of the invention
Below in conjunction with being embodied as safety, the present invention will be further described in detail, but the present invention is not limited to following example, the implementation condition adopted in embodiment can do further adjustment according to specifically used different requirement, and not marked implementation condition is the condition in normal experiment.
Embodiment 1, Caulis Spatholobi red pigment absorption spectrum mensuration
1, preparation Caulis Spatholobi powder
The Caulis Spatholobi of drying is cut into slices and pulverizes, take 100 order powder stand-by.
2, the mensuration of Caulis Spatholobi red pigment absorption spectrum
Weigh 1.0g Caulis Spatholobi powder, put in the conical flask of existing 30ml extracting solution, with 3min centrifugal under 3000r/min after lixiviate 2h at 60 DEG C, red pigment supernatant is diluted 40 times, full wavelength scanner under 320nm-800nm, the maximum absorption wavelength obtaining Caulis Spatholobi red pigment is 340nm.
Caulis Spatholobi red pigment solution is that 340nm and 460nm place crest occurs at wavelength, has obtained the maximum absorption at 340nm, and is gradually reduced along with the increase of wavelength.Therefore, the light absorption value size that index is 340nm place that Caulis Spatholobi red pigment technique is good and bad is extracted in this experiment.
Embodiment 2, extractant volume fraction of ethanol select impact on extraction effect
Weigh 5 parts of 1.0g Caulis Spatholobi powder, be respectively put in 5 conical flasks.In conical flask, add the 0% of 30mlpH=2 respectively, 20%, 40%, 60%, 80% ethanol extract.After being sufficiently stirred for, it is placed in Ultrasound Instrument, at constant temperature 60 DEG C, extracts 30min.Then being taken out by lixiviating solution, under 3000r/min, centrifugal 3min, dilutes 40 times by red pigment supernatant, measures its light absorption value when maximum absorption wavelength 340nm.Design three parallel tests.
As it is shown in figure 1, when the concentration of alcohol of extractant increases, light absorption value increases therewith, crest occurs when concentration of alcohol is 60%, and after 60% concentration of alcohol, the light absorption value of extracting solution begins to decline.Therefore, optimum extraction effect is 60% ethanol extraction agent.
Embodiment 3, the pH impact on extraction effect
Weigh 6 parts of 1.0g Caulis Spatholobi powder, be respectively put in 6 conical flasks.60% ethanol extract of 30mlpH=0,2,4,6,8,10 is added respectively in conical flask.After being sufficiently stirred for, it is placed in Ultrasound Instrument, at constant temperature 60 DEG C, extracts 30min.Then being taken out by lixiviating solution, under 3000r/min, centrifugal 3min, dilutes 40 times by red pigment supernatant, measures its light absorption value when maximum absorption wavelength 340nm.Design three parallel tests.
As in figure 2 it is shown, when pH is gradually increased, the light absorption value of extracting solution shows as first to raise and declines afterwards, is finally at plateau.When pH2, light absorption value reaches maximum.The light absorption value that other pH value extract gained is less, it may be possible to pH is relatively big to the stability influence of Caulis Spatholobi red pigment, and therefore, optimum extraction liquid pH value is 2.
Embodiment 4, solid-liquid ratio are on the impact of red pigment extraction ratio in Caulis Spatholobi
Weigh 5 parts of 1.0g Caulis Spatholobi powder, be respectively put in 5 conical flasks.60% ethanol extract of 10ml, 20ml, 30ml, 40ml, 50mlpH=2 it is separately added in each conical flask.After being sufficiently stirred for, it is placed in Ultrasound Instrument, at constant temperature 60 DEG C, extracts 30min.Then being taken out by lixiviating solution, under 3000r/min, centrifugal 3min, dilutes 40 times by red pigment supernatant, measures its light absorption value when maximum absorption wavelength 340nm.Design three parallel tests.
As it is shown on figure 3, when solid-liquid ratio increases, light absorption value then increases therewith.There is peak value at 1:40 place in solid-liquid ratio, then begins to reduce.Therefore, this experiment optimum extraction solid-liquid ratio is 1:40 (g/ml).
The impact on extraction effect of embodiment 5, ultrasonic treatment time
Weigh 5 parts of 1.0g Caulis Spatholobi powder, be respectively put in 5 conical flasks.Add the 60% ethanol extract 30ml of pH=2 under the same conditions.After being sufficiently stirred for, it is placed in Ultrasound Instrument, at constant temperature 60 DEG C, extracts 10min, 20min, 30min, 40min, 50min respectively.Then being taken out by lixiviating solution, under 3000r/min, centrifugal 3min, dilutes 40 times by red pigment supernatant, measures its light absorption value when maximum absorption wavelength 340nm.Design three parallel tests.
As shown in Figure 4, during prolongation between upon extracting, light absorption value increases therewith, but, extraction time, pigment extraction ratio was substantially at invariant state after 30min, this is likely due to extracting solution between at this moment has been saturation, or in Caulis Spatholobi sample, red pigment major part is extracted.Therefore, best extraction time is 30min.The Best Times 90min being considerably less than in document required for restricted-access media.
The impact on extraction effect of embodiment 6, temperature
Weigh 5 parts of 1.0g Caulis Spatholobi powder, be respectively put in 5 conical flasks.Add the 60% ethanol extract 30ml of pH=2 under the same conditions.After being sufficiently stirred for, it is placed in Ultrasound Instrument, regulates extraction 30min at the temperature of 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C respectively.Then being taken out by lixiviating solution, under 3000r/min, centrifugal 3min, dilutes 40 times by red pigment supernatant, measures its light absorption value when maximum absorption wavelength 340nm.Design three parallel tests.
As it is shown in figure 5, when Extracting temperature increases, extracting solution light absorption value increases therewith, but when 80 DEG C, color substantially deepens, and muddiness occurs.It is likely due to hot conditions and accelerates metachromasia.This characteristic is generally more stable with natural pigment character when low temperature, heating or high temperature can be accelerated metachromatic feature and be consistent, so red pigment is had destructiveness by high temperature, therefore, this experiment thinks that the pigment extracted at 80 DEG C is unavailable, and best Extracting temperature is 70 DEG C.
The orthogonal test that embodiment 7, Caulis Spatholobi red pigment extract
According to experiment of single factor result, design the L with four factors such as solid-liquid ratio, temperature, time, concentration of alcohol9(34) four factor three horizontal quadratures test, and design three parallel, average.Specifically determining Caulis Spatholobi red pigment ultrasonic extraction optimum process, design experiment factor level is in Table 1.
Table 1 orthogonal test factor level table
Result is as shown in table 2.In solid-liquid ratio, temperature, extraction time, four factors of concentration of alcohol, Caulis Spatholobi red pigment extraction ratio is affected size order is: solid-liquid ratio > temperature > time > concentration of alcohol.Optimum extraction process is test 3, and namely the extraction effect best conditions of extracting solution is: solid-liquid ratio 1:30, temperature 70 C, extraction time 50min, 70% concentration of alcohol.And by after range analysis, it has been found that the optimum combination that red pigment extracts is: solid-liquid ratio 1:30, temperature 70 C, extraction time 50min, 50% concentration of alcohol.
Table 2 Caulis Spatholobi red pigment extracts orthogonal experiments
By table 3 variance analysis it can be seen that Caulis Spatholobi red pigment extraction effect is had significant (P < 0.05) by solid-liquid ratio, other factors are not notable.
Table 3 the results of analysis of variance
Note: * represents notable, and * * represents highly significant, F0.05(2,4)=6.940
Embodiment 8, checking test
Because the technique that orthogonal experiments finds with range analysis is not inconsistent, therefore both contrast experiments of design, to further determine that the optimised process using ultrasonic assistant method to extract Caulis Spatholobi red pigment.The optimised process of orthogonal test is 70% concentration of alcohol of pH=2, solid-liquid ratio 1:30, temperature 70 C, extraction time 50min.The technique that range analysis finds is: 50% concentration of alcohol of pH=2, solid-liquid ratio 1:30, temperature 70 C, extraction time 50min.
Test result indicate that: the light absorption value of the technique using range analysis to find is more stable, and light absorption value has reached 0.802, and the light absorption value of orthogonal test optimised process is 0.778.Therefore this test thinks that ultrasonic assistant method extracts the extracting solution of 50% concentration of alcohol of optimised process pH=2 of Caulis Spatholobi red pigment, solid-liquid ratio 1:30, temperature 70 C, extraction time 50min.
The impact on extraction effect of embodiment 9, extraction time
According to the optimum extraction process that orthogonal test obtains, Caulis Spatholobi red pigment is extracted repeatedly, until extracting solution is colourless, collect each extracting solution respectively, measure each extracting liquid volume (v) and absorbance (a), each extracting solution is merged to obtain cumulative volume (V) and total light absorption value (A), and extraction ratio is calculated as follows:
Extraction ratio=(v × a)/(V × A) × 100%
As shown in Figure 6, when extracting the 3rd time, extraction rate reached is to 97.7% for result, higher than 95%, illustrates that major part pigment is extracted.When extracting the 4th, extracting solution is for clarifying, and extraction ratio when illustrating to extract the 4th has been 100%.Therefore, this test is to extract 3 times for best.
The ultrasonic assistant of the present invention extracts the method for Caulis Spatholobi pigment, extracting solution pH, concentration of alcohol are investigated, Caulis Spatholobi pigment is extracted the impact of result by solid-liquid ratio, ultrasonic temperature, ultrasonic time and extraction time, pass through orthogonal test, obtaining ultrasonic assistant and extract the best approach of Caulis Spatholobi pigment, the method extraction efficiency is high, saves solvent, simple to operate, it is convenient to extract.
Although have been presented for some embodiments of the present invention herein, it will be appreciated by those of skill in the art that without departing from the spirit of the invention, it is possible to the embodiments herein is changed.Above-described embodiment is illustrative of, should restriction using the embodiments herein as interest field of the present invention.
Claims (9)
1. the method that a ultrasonic assistant extracts Caulis Spatholobi pigment, it is characterised in that take Caulis Spatholobi section, crushed after being dried, obtain Caulis Spatholobi powder；With ethanol for extracting solution, after stirring, supersound extraction.
2. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that described Caulis Spatholobi powder size is 100 orders.
3. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that in described ethanol extract, concentration of alcohol is 40～80%.
4. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that described ethanol extract pH=1～4.
5. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that described supersound extraction temperature is 40～80 DEG C.
6. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that the described supersound extraction time is 30～50min.
7. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that described Caulis Spatholobi powder and ethanol extract solid-liquid ratio are 1:30～1:50.
8. the method that a kind of ultrasonic assistant as claimed in claim 1 extracts Caulis Spatholobi pigment, it is characterised in that take Caulis Spatholobi section, crushed after being dried, obtain Caulis Spatholobi powder；With the solid-liquid ratio of 1:30, adding the ethanol extract of pH=2 in described Caulis Spatholobi powder, in described ethanol extract, concentration of alcohol is 50%；After being sufficiently stirred for, 70 DEG C of supersound extraction 50min；Described ultrasonic power is 40KHz.
9. the method that a kind of ultrasonic assistant as claimed in claim 8 extracts Caulis Spatholobi pigment, it is characterised in that described supersound extraction number of times is 3 times.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106189356A (en) * | 2016-08-19 | 2016-12-07 | 南丹绣玉工艺品有限公司 | Vegetable colour |
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| CN1995151A (en) * | 2006-12-27 | 2007-07-11 | 浙江理工大学 | Spatholobus stem natural dye preparation and its uses |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1995151A (en) * | 2006-12-27 | 2007-07-11 | 浙江理工大学 | Spatholobus stem natural dye preparation and its uses |
Non-Patent Citations (4)
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| 刘海花等: "《鸡血藤红色素的提取及其稳定性研究》", 《检验医学教育》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106189356A (en) * | 2016-08-19 | 2016-12-07 | 南丹绣玉工艺品有限公司 | Vegetable colour |
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Application publication date: 20160713 |