CN103472056B - Purple sweet potato anthocyanin measures the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin - Google Patents
Purple sweet potato anthocyanin measures the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin Download PDFInfo
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- CN103472056B CN103472056B CN201310433406.4A CN201310433406A CN103472056B CN 103472056 B CN103472056 B CN 103472056B CN 201310433406 A CN201310433406 A CN 201310433406A CN 103472056 B CN103472056 B CN 103472056B
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Abstract
The invention discloses a kind of purple sweet potato anthocyanin and measure the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin, purple sweet potato anthocyanin that what the present invention set up utilize to substitute in GB6195-1986 2,6-dichloroindophenol, measure the feature that method has safely, cheap, accuracy is suitable with 2,6-dichloroindophenol method titrimetry of Vitamin C content in fruit, vegetables.Preparation method of the present invention comprise salt acid soak, concentration, cross post purifying, purple sweet potato anthocyanin the step such as to produce.Because chemical reagent used in leaching process only has φ (HCl) to be the hydrochloric acid solution of 0.2%, so whole extraction process almost not polluting environment, security is high.
Description
Technical field
The present invention relates to a kind of preparation method of pigment, particularly relate to a kind of purple sweet potato anthocyanin and measure the method for fruits and vegetables vitamin and the preparation method of purple sweet potato anthocyanin.
Background technology
Purple potato (formal name used at school: Ipomoeabatatas) is again black potato, potato meat be purple to darkviolet, be rich in protein, starch, pectin, vitamin and several mineral materials, also contain anthocyanidin simultaneously.In the purple potato of general maturation, the content of anthocyanidin (Anthocyanidin) class pigment is 0.2-0.8%, and some kind can up to 1.2%.The domestic and international extraction to purple sweet potato anthocyanin and physiologically active have carried out a series of research, about the molecular structure of this type of pigment and the research of component analysis also make some progress.Purple potato pigment is soluble in water, belong to non-fat-soluble pigment, its existence form is anthocyanin, anthocyanin is the compound that anthocyanidin (anthocyanidin) is combined into glycosidic bond with sugar, as glucopyranoside Cyanidin and peonidin, the agent structure pyranoid ring in purple sweet potato anthocyanin pigment there is a tetravalence oxygen atom.But the applied research of serving as oxygenant about purple sweet potato anthocyanin does not also appear in the newspapers.
GB6195-1986 is National Standard of the People's Republic of China's fruit, vegetables Vitamin C content determination method (2,6-dichloroindophenol titrimetry).The method main agents 2,6-dichloroindophenol used is organic synthesis pigment, expensive, and can stimulate the eyes of human body, respiratory tract and skin.
Therefore, the present invention, according to the fundamental characteristics of anthocyanidin, utilizes hydrochloric acid solution infusion method to extract from purple potato and prepares anthocyanidin, analyzes it and replaces 2,6-dichloroindophenol quantitative measurement fruit, the ascorbic effect of vegetables used in GB6195-1986.Purple sweet potato anthocyanin has aboundresources, advantage that security is good.
Summary of the invention
One object of the present invention is that the purple sweet potato anthocyanin providing a kind of abundant raw material source, production cost lower measures the method for fruits and vegetables vitamin.
Another object of the present invention is the preparation method of the purple sweet potato anthocyanin providing a kind of security high.
For achieving the above object, technical solution of the present invention is:
The present invention is a kind of method that purple sweet potato anthocyanin measures fruits and vegetables vitamin, and it uses purple sweet potato anthocyanin as quantitative measurement fruit, the ascorbic reagent of vegetables.
The present invention is a kind of preparation method of purple sweet potato anthocyanin, and it comprises the following steps: (1) salt acid soak: by clean purple potato stripping and slicing, pulverizing, and the solution adding hydrochloric acid volume fraction φ (HCl) 0.1-0.3% soaks; (2) concentration: centrifugal treating contains the hydrochloric acid solution soak solution of purple potato, obtains supernatant, is pigment crude extract; Pigment crude extract is contained in beaker, is placed in the unlimited evaporation of thermostat water bath and concentrates, obtain concentrate; (3) cross post purifying: concentrate is crossed SephadexG-25 post and carry out purifying, collect filtered fluid, again concentration; (4) the producing of purple sweet potato anthocyanin: dry at 55-65 DEG C, obtain purple sweet potato anthocyanin, yield is the purple potato of 0.65g anthocyanidin/100g.
The individual weight of described purple potato is 250 ± 50g.
Its volume fraction of hydrochloric acid solution used in step (1) is 0.2%, and the ratio of purple potato and hydrochloric acid solution is 1:15-25, and namely the purple potato of 1g adds the hydrochloric acid solution of 15 ~ 25mL0.2%.
In step (1), salt acid soak is under the water bath condition of 40-60 DEG C, stirs again and extracts 2h, during stirring, stir 1min every 15min after first soaking 1h.
Concentration described in step (2) carries out opening wide in thermostat water bath concentrating, temperature 80 DEG C, time 12h.
In step (3), the chromatographic column of purifying is SephadexG-25 post, and eluant, eluent is the solution of hydrochloric acid volume fraction φ (HCl) 0.2%.
After adopting such scheme, because the present invention contains anthocyanidin according to purple potato, this anthocyanidin is soluble in water, belong to the characteristic of non-fat-soluble pigment, adopt hydrochloric acid solution immersing extraction pigment, concentration is opened wide concentrated in the thermostat water bath of 80 DEG C, the pigment loss caused due to the saponins evaporation easy to foaming existed in purple potato when avoiding traditional reduced pressure concentration, and utilize the Stationary liquid purifying pigment with molecular sieve character, improve the yield of pigment.The pigment prepared is the bronzing pigment of paste.This pigment can replace ascorbic content in 2,6-dichloroindophenol quantitative measurement fruit used in GB6195-1986, vegetables.
Because chemical reagent used in leaching process only has hydrochloric acid volume fraction φ (HCl) to be the solution of 0.2%, so whole extraction process almost not polluting environment.Therefore the present invention has the following advantages:
1, the present invention utilizes purple potato as raw material, and abundant raw material source, cost are low.
2, the pigment yield of the present invention's extraction is high, and the purple potato of every 100g can obtain 0.65g anthocyanidin.
3, the pigment that prepared by the present invention has oxidized and reduced two kinds of existences.When this pigment serves as oxygenant, electronics can be obtained from reductive agent, the quantivalency of the tetravalence oxygen atom on the agent structure pyranoid ring in anthocyani pigment is reduced.
4, the present invention prepare pigment oxidation state time, be red in acid medium, be blue-green in alkali condition; Be colourless when reduction-state.
5, after the pigment that prepared by the present invention substitutes 2,6-dichloroindophenols in GB6195-1986, the preci-sion and accuracy of assay method can meet the requirement of assay method.
In sum, what the present invention set up utilizes purple sweet potato anthocyanin to substitute 2,6-dichloroindophenols in GB6195-1986, measures the feature that method has safely, cheap, accuracy is suitable with 2,6-dichloroindophenol method titrimetry of Vitamin C content in fruit, vegetables.
Below in conjunction with body embodiment, the present invention is further illustrated.
Embodiment
One, assay method
The present invention is a kind of method that purple sweet potato anthocyanin measures fruit and vegetable vitamin C, and it uses purple sweet potato anthocyanin as quantitative measurement fruit, the ascorbic reagent of vegetables.
(1) feature of purple sweet potato anthocyanin: this anthocyanidin has characteristic absorption peak at 530nm place, and molecular weight ranges is between 850 ~ 1020u.In 200-700nm wavelength coverage, dilution is slightly carried to pigment and carry out spectral scan, determine that this anthocyanidin has characteristic absorption peak at 530nm place, adopt molecular exclusion chromatography to measure the molecular weight ranges of this pigment between 850 ~ 1020u.
(2) pigment to substitute in GB6195-1986 2, the reason of 6-dichloroindophenol: purple sweet potato anthocyanin has oxidized and reduced two kinds of existences, its color depends on its redox state, oxidation state is red in acid medium, it is blue-green in alkali condition, reduction-state becomes colorless, and is through and Na
2sO
3and H
2o
2the result gained of solution reaction, the color feature of 2,6-dichloroindophenols in this and GB6195-1986 is similar.This pigment is red in oxidation state in acid medium, be blue-green in alkali condition, be observe different pH value damping fluid on the damp result affecting gained of pigmentary color.Described Precision Experiment result, use 2, relative standard deviation during 6-dichloroindophenol titrimetry is 1.43%, purple sweet potato anthocyanin method relative standard deviation when using this pigment is 1.47%, all be less than 2%, it is feasible that explanation purple sweet potato anthocyanin substitutes 2,6-dichloroindophenols in GB6195-1986, and after substituting, repeatability is high.Accuracy experimental result: use purple sweet potato anthocyanin titrimetry recovery during this pigment 95.4 ~ 98.6%, average recovery rate is 97.4%, RSD is 1.20%; The recovery of 2,6-dichloroindophenol titrimetry is 96.5 ~ 98.7%, and average recovery rate is 97.6%, RSD is 0.87%.The result of two kinds of method mensuration is very close.
(3) pigment substitutes 2 in GB6195-1986, to measure in summer orange and tomato ascorbic content in the result of ascorbic content: Xia Cheng and tomato after 6-dichloroindophenol and be respectively (25.33 ± 0.34) mg/100g, (20.41 ± 0.32) mg/100g; And 2,6-dichloroindophenol titration measuring summers are orange and in tomato, ascorbic content is respectively (25.28 ± 0.46) mg/100g, (20.25 ± 0.21) mg/100g.
Two, preparation method
The present invention is a kind of preparation method of purple sweet potato anthocyanin, and it comprises the following steps:
Embodiment 1:
(1) salt acid soak: by purple potato cleaning, peeling, stripping and slicing (thickness is about 2cm), with stirrer making beating process of squeezing the juice to pulverizing to obtain purple potato end.Get the purple potato end of 50g, add hydrochloric acid volume fraction φ (HCl) 0.2% solution of 1L, under the water bath condition of 40 DEG C, soak 1h, then stir extraction 2h(every 15min, stir 1min), centrifugal 5min under 4000r/min, obtains supernatant, i.e. pigment crude extract.
(2) concentration: by the pigment crude extract obtained, be contained in the beaker of 5 300mL, is placed in the unlimited evaporation of 80 DEG C of thermostat water baths and concentrates, obtain concentrate.
(3) post purifying is crossed: by the concentrate of acquisition through SephadexG-25 post (3.0cm × 60cm), applied sample amount 3.0mL, carries out wash-out, flow velocity 2mL/min with hydrochloric acid volume fraction φ (HCl) 0.2% solution, eluent collected by automatic portion collection instrument, and often 2mL collected by pipe.Repeat 10 times, merging color is mauve eluent, again opens wide the pigment solution that evaporation obtains purifying.
(4) preparation of purple sweet potato anthocyanin: the pigment solution of purifying is placed in baking oven dry (60 DEG C of 3h), obtains the purple potato of 0.35g anthocyanidin goods/50g.
Embodiment 2
(1) salt acid soak: by purple potato cleaning, peeling, stripping and slicing (thickness is about 1cm), with stirrer making beating process of squeezing the juice to pulverizing to obtain purple potato end.Get the purple potato end of 25g, add hydrochloric acid volume fraction φ (HCl) 0.1% solution of 0.375L, under the water bath condition of 50 DEG C, soak 2h, then stir extraction 1h(every 15min, stir 1min), centrifugal 5min under 4500r/min, obtains supernatant, i.e. pigment crude extract.
(2) concentration: by the pigment crude extract obtained, be contained in the beaker of 3 300mL, is placed in the unlimited evaporation of 70 DEG C of thermostat water baths and concentrates, obtain concentrate.
(3) post purifying is crossed: by the concentrate of acquisition through SephadexG-25 post (3.0cm × 65cm), applied sample amount 3.5mL, carries out wash-out, flow velocity 2mL/min with hydrochloric acid volume fraction φ (HCl) 0.2% solution, eluent collected by automatic portion collection instrument, and often 2.5mL collected by pipe.Repeat 6 times, merging color is mauve eluent, again opens wide the pigment solution that evaporation obtains purifying.
(4) preparation of purple sweet potato anthocyanin: the pigment solution of purifying is placed in baking oven dry (55 DEG C of 4h), obtains the purple potato of 0.15g anthocyanidin goods/25g.
Embodiment 3
(1) salt acid soak: by purple potato cleaning, peeling, stripping and slicing (thickness is about 2cm), with stirrer making beating process of squeezing the juice to pulverizing to obtain purple potato end.Get the purple potato end of 75g, add hydrochloric acid volume fraction φ (HCl) 0.3% solution of 1.875L, under the water bath condition of 60 DEG C, soak 1h, then stir extraction 2h(every 15min, stir 1min), centrifugal 5min under 4000r/min, obtains supernatant, i.e. pigment crude extract.
(2) concentration: by the pigment crude extract obtained, be contained in the beaker of 7 300mL, is placed in the unlimited evaporation of 80 DEG C of thermostat water baths and concentrates, obtain concentrate.
(3) post purifying is crossed: by the concentrate of acquisition through SephadexG-25 post (3.0cm × 67cm), applied sample amount 3.5mL, carries out wash-out, flow velocity 2mL/min with hydrochloric acid volume fraction φ (HCl) 0.2% solution, eluent collected by automatic portion collection instrument, and often 3mL collected by pipe.Repeat 15 times, merging color is mauve eluent, again opens wide the pigment solution that evaporation obtains purifying.
(4) preparation of purple sweet potato anthocyanin: the pigment solution of purifying is placed in baking oven dry (65 DEG C of 3h), obtains the purple potato of 0.54g anthocyanidin goods/75g.
What the present invention set up utilizes purple sweet potato anthocyanin to substitute 2,6-dichloroindophenols in GB6195-1986, measures the feature that method has safely, cheap, accuracy is suitable with 2,6-dichloroindophenol method titrimetry of Vitamin C content in fruit, vegetables.
Emphasis of the present invention is just: utilize purple sweet potato anthocyanin to substitute 2,6-dichloroindophenols in GB6195-1986, measures Vitamin C content in fruit, vegetables.
Above are only specific embodiments of the invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading scope.
Table 1 summer that double methods of titration is surveyed orange and tomato in ascorbic content (n=6)
Table 2 double methods of titration recovery of standard addition measurement result
Claims (7)
1. purple sweet potato anthocyanin measures a method for fruits and vegetables vitamin, it is characterized in that: it uses purple sweet potato anthocyanin as quantitative measurement fruit, the ascorbic oxygenant of vegetables.
2. the preparation method of a purple sweet potato anthocyanin according to claim 1, it is characterized in that: it comprises the following steps: (1) salt acid soak: by clean purple potato stripping and slicing, pulverizing, the solution adding volume fraction φ (HCl) 0.1-0.3% of hydrochloric acid soaks; (2) concentration: centrifugal treating contains the hydrochloric acid solution soak solution of purple potato, obtains pigment crude extract; Pigment crude extract is contained in beaker, is placed in the unlimited evaporation of thermostat water bath and concentrates, obtain concentrate; (3) cross post purifying: concentrate is crossed SephadexG-25 post and carry out purifying, collect filtered fluid, again concentration; (4) the producing of purple sweet potato anthocyanin: dry at 55-65 DEG C, obtain purple sweet potato anthocyanin.
3. the preparation method of purple sweet potato anthocyanin according to claim 2, is characterized in that: the individual weight of described purple potato is 250 ± 50g.
4. the preparation method of purple sweet potato anthocyanin according to claim 2, is characterized in that: its volume fraction of hydrochloric acid solution used in step (1) is 0.2%, and the ratio of purple potato and hydrochloric acid solution is 1:15-25.
5. the preparation method of purple sweet potato anthocyanin according to claim 2, is characterized in that: in step (1), salt acid soak is under the water bath condition of 40-60 DEG C, stirs again and extracts 2h, during stirring, stir 1min every 15min after first soaking 1h.
6. the preparation method of purple sweet potato anthocyanin according to claim 2, is characterized in that: the concentration described in step (2) carries out opening wide in thermostat water bath concentrating, temperature 80 DEG C, time 12h.
7. the preparation method of purple sweet potato anthocyanin according to claim 2, is characterized in that: in step (3), the chromatographic column of purifying is SephadexG-25 post, and eluant, eluent is the solution of the volume fraction φ (HCl) 0.2% of hydrochloric acid.
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| CN103880804B (en) * | 2014-03-20 | 2015-12-02 | 江苏大学 | A kind of method of anthocyanidin in extraction and isolation purple sweet potato powder |
| CN107382949A (en) * | 2017-08-29 | 2017-11-24 | 贵州省苗岭经济林技术开发有限公司 | A kind of purple potato wine brewing extraction purple sweet potato anthocyanin method |
| CN108732298A (en) * | 2018-07-26 | 2018-11-02 | 青岛科技大学 | It is a kind of detection blueberry anthocyanidin content method and application |
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| CN103160139A (en) * | 2011-12-08 | 2013-06-19 | 上海蓝普生物科技有限公司 | Extraction method for natural pigment |
| WO2013086621A1 (en) * | 2011-12-16 | 2013-06-20 | CENTRE DE RECHERCHE INDUSTRIELLE DU QUéBEC | Method for extracting anthocyanin derivatives from a plant source |
| CN102432582A (en) * | 2011-12-29 | 2012-05-02 | 广西金宏昕生物科技有限公司 | Preparation method of proanthocyanidin |
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