CN105062133A - Method for extracting anthocyanidin from syzygium samarangense peel - Google Patents
Method for extracting anthocyanidin from syzygium samarangense peel Download PDFInfo
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- CN105062133A CN105062133A CN201510572569.XA CN201510572569A CN105062133A CN 105062133 A CN105062133 A CN 105062133A CN 201510572569 A CN201510572569 A CN 201510572569A CN 105062133 A CN105062133 A CN 105062133A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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Abstract
The invention discloses a method for extracting anthocyanidin from syzygium samarangense peel. The method specifically comprises the following steps of peeling mature syzygium samarangense fruits by virtue of a peeler, crushing the peel, adding an extracting solution prepared by mixing citric acid-absolute ethyl alcohol according to a material-to-liquid ratio of 1:50, and performing extraction for 40 minutes at 50 DEG C. According to the method, anthocyanidin in the syzygium samarangense peel can be effectively extracted, the extraction rate can reach 12.950mg/100g, blanks in researches and utilization of syzygium samarangense peel are filled, the obtained anthocyanidin can further be used as a natural pigment, and a new approach for the development and the utilization of fruit and vegetable anthocyanidin is provided.
Description
Technical field
The invention belongs to deep-processing technical field of agricultural products, be specifically related to the extracting method of cyanidin(e) in a kind of wax-apple pericarp.
Background technology
Food dye can be divided into natural pigment and the large class of chemical industry synthetic colour two.Synthetic colour because it is cheap, the characteristic such as stable, easy coloring is widely used in modern food industry, but much research shows that it has the harm such as the normal function of carcinogenic, infringement subcellular human structure, interference various active enzyme.And natural pigment has the biological activity such as anti-oxidant, scavenging free radicals, anti-mutation, anticancer, antiviral, lipopenicillinase, plays a crucial role in preventing cardiovascular disease, diabetes and cancer.Therefore, the applicating and exploitation of natural pigment more and more receives publicity and payes attention to.
Wax-apple (
syzygium.samarangense(BI.) Merr.etPerry) be emerging tropical fruit tree, fresh fruit price is high, and its heat affected zone orchard worker is liked, very fast in hot-zone development in recent years.The different colours such as wax-apple fruit maturation fruit in season leatherware is dark red, pink, dark green, white, are wherein all rich in anthocyanin when pink kind and dark red kind of fruit maturation, be the good material of exploitation natural pigment.Have at present and the extraction of cyanidin(e) in the fruits and vegetables such as purple potato, grape is studied, but also do not have the report that the exploitation of cyanidin(e) in wax-apple are studied.
Summary of the invention
The object of the present invention is to provide the extracting method of cyanidin(e) in a kind of wax-apple pericarp, to make up the blank of cyanidin(e) research and utilization in current wax-apple pericarp, the exploitation for fruits and vegetables class cyanidin(e) provide a new way.
For achieving the above object, the present invention adopts following technical scheme:
The extracting method of cyanidin(e) in a kind of wax-apple pericarp, its concrete steps are: get ripe wax-apple fruit, surface-moisture is dried after cleaning, pericarp is dug with planing tool, then by pericarp in crusher for crushing, add extracting solution lixiviate 1-2 time by solid-liquid ratio 1:50 pericarp after being pulverized again, extraction temperature is 50 DEG C, each lixiviate 40min.
The fruit colour of described ripe wax-apple fruit is scarlet or pink; Described wine-colored lustre index is L(luminance index): 15 ~ 35, ho(colourity angle): 2 ~ 5, a(red green index): 15 ~ 30, b(champac index): 1.5 ~ 3.5; Described peach lustre index is L:40 ~ 60, ho:10 ~ 20, a:30 ~ 50, b:7 ~ 10.
Extracting solution used is mixed citric acid and dehydrated alcohol; In extracting solution, the mass concentration of citric acid is 2.5%.
remarkable advantage of the present invention is: the inventive method is simple, with low cost, and effectively can extract the cyanidin(e) in wax-apple pericarp, its extraction yield can reach 12.950mg/100g, can realize preparation and suitability for industrialized production on a small scale; And extracting solution used is simple and easy to get, non-toxic and safe, can keep the stability of cyanidin(e) preferably.
The present invention compensate for the blank of cyanidin(e) research and utilization in current wax-apple pericarp, and gained cyanidin(e) can be further used as natural pigment and use, and the exploitation for fruits and vegetables class cyanidin(e) provide a new way.
Accompanying drawing explanation
Fig. 1 is the impact of different extracting solution on extraction effect.
Fig. 2 be in extracting solution different ethanol concentration on the impact of extraction effect.
Fig. 3 is the impact of different ultrasonic power on extraction effect.
Fig. 4 is that different extraction time is on the impact of extraction effect.
Fig. 5 is the impact of different Extracting temperature on extraction effect.
Fig. 6 is the impact of different feed liquid comparison extraction effect.
Fig. 7 is the impact of different extraction time on extraction effect.
Note: in figure, capitalization difference represents that difference extremely significantly (P<0.01), and lowercase difference represents significant difference (P<0.05), and same letter represents difference not significantly (P>0.05).
Embodiment
More being convenient to make content of the present invention understand, below in conjunction with embodiment, technical solutions according to the invention are described further, but the present invention being not limited only to this.
1 materials and methods
1.1 material
Be that (its lustre index is for L:15 ~ 35 for test materials with ' purplish red ' wax-apple mature fruit pericarp, ho:2 ~ 5, a:15 ~ 30, b:1.5 ~ 3.5), pick up from Zhangzhou City's Dongshan County circle and send out wax-apple plantation, dry surface-moisture after cleaning, dig pericarp with planing tool, then that pericarp is for subsequent use in crusher for crushing.
Hydrochloric acid, methyl alcohol, dehydrated alcohol, citric acid, acetone etc. are analytical reagent.Key instrument is Lambda35 ultra-violet and visible spectrophotometer (PerkinElmer limited-liability company), SK5210 ultrasonic cleaner (Shanghai High Kudos Science Instrument Co., Ltd.), pulverizer, XMTD-8222 water-bath (the upper grand experimental installation company limited of Nereid) etc.
1.2 method
1.2.1 single factor experiment
Take a certain amount of wax-apple pericarp, by the extracting solution of single factor design, extract concentration, ultrasonic power, extraction time, Extracting temperature, solid-liquid ratio, wax-apple pericarp is extracted.The extraction efficiency of each extracting solution represents with cyanidin(e) content:
Anthocyanin content (mg/100g)=A × V × 1000 × 455.2 × 100/29600 × d × m,
In formula: A: maximum absorption wave strong point absorbance; V: constant volume (L); 1000:g is converted into the number that mg expands; 455.2: the molecular mass (g/mol) of Cy-3-G; 29600: the concentration ratio uptake factor (L/molcm) of Cy-3-G; D: cuvette optical path (cm); M: Fresh Yuxincao (g).
1.2.1.1 extracting solution is on the impact of extraction effect
Take 8 parts of wax-apple pericarps in 15mL centrifuge tube, every part of 5g, add A:1% hydrochloric acid-methanol (pH2.65), B:1% hydrochloric acid-dehydrated alcohol (pH2.71), C:2.5% citric acid-methyl alcohol (w/v respectively, pH2.65), D:2.5% citric acid-dehydrated alcohol (w/v, pH2.85), E:1% hydrochloric acid-95% ethanol (pH3.01), F: methyl alcohol (pH6.98), G: dehydrated alcohol (pH7.02), each 10mL of H:80% acetone (pH7.01) extracting solution, 100W power ultrasonic lixiviate 30min at 30 DEG C, after filtering, filtrate is settled to 25mL.
1.2.1.2 in extracting solution different ethanol concentration on the impact of extraction effect
Take 6 parts of wax-apple pericarps in 15mL centrifuge tube, every part of 5g, add 10mL2.5% citric acid-dehydrated alcohol, 2.5% citric acid-90% ethanol, 2.5% citric acid-80% ethanol, 2.5% citric acid-70% ethanol, 2.5% citric acid-60% ethanol, 2.5% citric acid-50% ethanol respectively, 100W power ultrasonic lixiviate 30min at 30 DEG C, after filtering, filtrate is settled to 25mL.
1.2.1.3 ultrasonic power is on the impact of extraction effect
Take 5 parts of wax-apple pericarps in 15mL centrifuge tube, every part of 5g, respectively add 10mL2.5% citric acid-dehydrated alcohol, respectively at 0W, 80W, 120W, 160W, 200W power ultrasonic lixiviate 30min at 30 DEG C, after filtering, filtrate is settled to 25mL.
1.2.1.4 extraction time is on the impact of extraction effect
Take 6 parts of wax-apple pericarps in 15mL centrifuge tube, every part of 5g, respectively add 10mL2.5% citric acid-dehydrated alcohol, difference lixiviate 10min, 20min, 30min, 40min, 50min, 60min at 30 DEG C, after filtering, filtrate is settled to 25mL.
1.2.1.5 Extracting temperature is on the impact of extraction effect
Take 5 parts of wax-apple pericarps in 15mL centrifuge tube, every part of 5g, respectively add 10mL2.5% citric acid-dehydrated alcohol, respectively at lixiviate 40min at 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, after filtering, filtrate is settled to 25mL.
1.2.1.6 solid-liquid ratio is on the impact of extraction effect
Take 7 parts of wax-apple pericarps in 50mL centrifuge tube, every part of 1g, respectively with solid-liquid ratio (g:mL) 1:5,1:10,1:15,1:20,1:30,1:40,1:50, adds 2.5% citric acid-dehydrated alcohol, 40 DEG C of water-bath lixiviate 40min, after filtering, filtrate is settled to 50mL.
1.2.1.7 extraction time is on the impact of extraction effect
Take wax-apple pericarp 1g, 2.5% citric acid-dehydrated alcohol is added with solid-liquid ratio (g:mL) 1:30,40 DEG C of water-bath lixiviate 40min, 50mL is settled to after filtration, filter residue repeats extraction 3 times again, measure cyanidin(e) content in each filtrate respectively, calculate each cyanidin(e) extracting gained and account for the ratio that 4 times are extracted gained cyanidin(e) total amount.
1.2.2 orthogonal test
Get alcohol concn in extracting solution, extraction time, Extracting temperature, solid-liquid ratio 4 factors, each factor arranges 3 levels, does orthogonal test, and to determine its optimum extraction process, factor and level are in table 1.
The factor of table 1 orthogonal test and level
1.3 data analysis
Data acquisition MicrosoftExcel software carries out drawing and analyzing, and carries out Duncan's inspection with SPSS software.
2 results and analysis
2.1 single factor experiment results
2.1.1 extracting solution is on the impact of extraction effect
As shown in Figure 1, extracting solution D(2.5% citric acid-dehydrated alcohol) extraction efficiency the highest, cyanidin(e) content pole is significantly higher than other extracting solutions, is secondly C(2.5% citric acid-methyl alcohol).Under the same terms, extraction using alcohol efficiency is better than methyl alcohol, and methyl alcohol and acetone extraction efficiency are without significant difference; The low extraction efficiency of pH value is high, A(pH2.65) and C(pH2.65) extraction efficiency be all significantly higher than F(pH6.98), E(pH3.01) extraction efficiency is also significantly higher than G(pH7.02), this can may keep the stability of cyanidin(e) relevant with low pH.Extraction using alcohol excellent in efficiency, economical nontoxic, and citric acid is common food additive, so selective extraction liquid D is optimum extraction liquid.
2.1.2 in extracting solution different ethanol concentration on the impact of extraction effect
As shown in Figure 2, along with the reduction of alcohol concn, cyanidin(e) extracts and totally presents downtrending.The extraction efficiency of 100% ethanol and 90% ethanol is all significantly higher than other concentration process in pole, and the extraction efficiency of 100% ethanol and 90% ethanol is also in pole significant difference, and therefore in extracting solution, alcohol concn is advisable with 100%.
2.1.3 ultrasonic power is on the impact of extraction effect
As can be seen from Figure 3, the impact of ultrasonic power on wax-apple cyanidin(e) extraction efficiency is not remarkable.Though through the cyanidin(e) extraction efficiency of ultrasonication higher than without ultrasonication, all do not reach significant difference.Based on simplification extraction conditions principle, select 0W ultrasonic power.
2.1.4 extraction time is on the impact of extraction effect
As shown in Figure 4, cyanidin(e) extraction efficiency extends with extraction time and increases.Extraction time is when being 40 ~ 60min, when cyanidin(e) extraction efficiency is significantly higher than 10 ~ 30min.Between extraction time 40min, 50min and 60min, cyanidin(e) extraction efficiency is without significant difference, and extraction time is long uneconomical, and easily causes cyanidin(e) to decompose, and therefore, extraction time is advisable with 40min.
2.1.5 Extracting temperature is on the impact of extraction effect
Fig. 5 shows, along with the rising of Extracting temperature, cyanidin(e) extraction efficiency increases.But when temperature is elevated to 50 DEG C, cyanidin(e) extraction efficiency slowly declines along with the continuation rising of temperature, and this may stablize because high temperature be unfavorable for cyanidin(e), easily causes it to decompose, so Extracting temperature is advisable with 50 DEG C.
2.1.6 solid-liquid ratio is on the impact of extraction effect
As shown in Figure 6, cyanidin(e) content first increases along with the reduction of solid-liquid ratio, and reach maximum to cyanidin(e) content during 1:50, the reduction subsequently with solid-liquid ratio is on a declining curve, therefore solid-liquid ratio selects 1:50 to be advisable.
2.1.7 extraction time is on the impact of extraction effect
As shown in Figure 7, the cyanidin(e) content of 1 lixiviate can reach 77.60%, and pole is significantly higher than the content of other extraction, and the cyanidin(e) content of the 2nd lixiviate is also significantly higher than the 3rd, 4 time in pole, can adopt 2 lixiviates in thus producing.For raising the efficiency, in test, adopt 1 lixiviate.
2.2 orthogonal experiments
With alcohol concn, extraction time, Extracting temperature, solid-liquid ratio 4 factors in extracting solution, do the orthogonal test of 4 factor 3 levels, result is as shown in table 2.
Table 2 orthogonal test and testing data result
From range analysis result, alcohol concn, Extracting temperature and solid-liquid ratio are on the extraction effect tool remarkably influenced of wax-apple cyanidin(e), wherein the strongest influence factor is alcohol concn (P<0.01, F=17.9265), be secondly solid-liquid ratio and Extracting temperature (P<0.05) respectively.Optimal extract process is the 23rd combination in orthogonal test, namely with 2.5% citric acid-dehydrated alcohol for extracting solution, solid-liquid ratio 1:50, in 50 DEG C, lixiviate 40min effect is best.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. the extracting method of cyanidin(e) in wax-apple pericarp, is characterized in that: get ripe wax-apple fruit, dries surface-moisture, dig pericarp with planing tool after cleaning, then by pericarp in crusher for crushing, then the pericarp after pulverizing be placed in extracting solution carry out lixiviate.
2. the extracting method of cyanidin(e) in wax-apple pericarp according to claim 1, is characterized in that: the fruit colour of described ripe wax-apple fruit is scarlet or pink;
Described wine-colored lustre index is L:15 ~ 35, ho:2 ~ 5, a:15 ~ 30, b:1.5 ~ 3.5; Described peach lustre index is L:40 ~ 60, ho:10 ~ 20, a:30 ~ 50, b:7 ~ 10.
3. the extracting method of cyanidin(e) in wax-apple pericarp according to claim 1, it is characterized in that: in leaching process, the solid-liquid ratio pulverizing pericarp and extracting solution is 1:50.
4. the extracting method of cyanidin(e) in wax-apple pericarp according to claim 1, is characterized in that: extracting solution used is mixed citric acid and dehydrated alcohol; In extracting solution, the mass concentration of citric acid is 2.5%.
5. the extracting method of cyanidin(e) in wax-apple pericarp according to claim 1, it is characterized in that: extraction temperature is 50 DEG C, extracting times is 1-2 time, each 40min.
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| CN102863418A (en) * | 2011-07-07 | 2013-01-09 | 徐州市农家欢农业科技有限公司 | Process for ultrasonic extraction of anthocyanin of purple corn leaves |
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