Background technology
Diospyros in Ebenaceae (
ebenaceae) Diospyros (
disopyos KakiL.) perennial deciduous fruit tree, originate in China.China's persimmon cultivated area about 1,000 ten thousand mu, accounts for 89% of the total cultivated area in the whole world, nearly 3,000,000 tons of annual production, and wherein more than 95% is puckery persimmon, can not directly eat after adopting, and is mainly used in manufacturing dried persimmon or supplying to eat raw after process of taking away the puckery taste.
The main component of persimmon fruit astringent taste is the soluble tannin in persimmon fruit, therefore, judges the method for persimmon deastringent degree, except the sensory evaluation of people, mainly measures the soluble tannin content in persimmon fruit.In general, when soluble tannin content in persimmon fruit lower than 0.2% time (also have report lower than 0.5% time), the mouthfeel of people is not able to appreciate astringent sense.
In production, as supplied, the carbon dioxide eating the puckery persimmon in market raw takes away the puckery taste, ethanol takes away the puckery taste, the determination suitable collection period etc. of sweet persimmon, usually needs the degree of taking away the puckery taste judging persimmon, persimmon soluble tannin content is tasted and measured to mouthfeel except people, do not have other method.
In astringent persimmon fruit, contained tannin belongs to condensed tannin, and the topmost construction unit of such tannin is catechin.Due to tannin may be oxidized when extraction and isolation, the reaction such as dissociation and polymerization, assay method conventional at present has Forint phenol method, vanillin-sulfuric acid method, n-butanol hydrochloric acid method 4-di methyl amino cinnamaldehyde method etc.There is the shortcoming that assay method is loaded down with trivial details, the time is long in these methods, and mostly adopts absolute methanol as working media, and what have has particular/special requirement to instrument, and toxicity is large, cost is high, can not meet demand simple and quick to tannis determination on producing well.Therefore, persimmon need badly simply in producing, deastringency of persimmon deciding degree method fast and effectively.
At present about the patent report of persimmon focuses mostly in deastringent agent (persimmon deastringent agent, application number 200810113288.8; Persimmon acerbity-removing fresh-keeping agent containing attapulgite, application number 200910034481.7; A kind of persimmon acerbity-removing fresh-keeping agent containing and application process, application number 02104426.0), acerbity removing method (a kind of persimmon deastringent, protects crisp processing method, application number 201310334046.2; Persimmon protects crisp preservation method, application number 201210105381.0; A method for deastringency of persimmon, application number 201310078060. 0; A kind of persimmon deastringent processing method, application number 200410012226.X; A kind of persimmon deastringent protects crisp method, application number 03130838.4) and (a kind of device of deastringency of persimmon, the application number 201320111287.6 such as deastruingent device; A kind of fresh persimmon deastruingent device, application number 201210582985.4; Fruit takes away the puckery taste dress, application number 201120558087.6; Automatic temperature control adjustable gas acerbity removing method for persimmon and used acerbity removing cabin thereof, application number 200710057232.0; A kind of Puckery removing processor for persimmon, application number 200420016046.4).There are no simply, fast, effectively determining that about persimmon (judgement) takes away the puckery taste the patent of degree and bibliographical information.
Summary of the invention
The present invention is directed to above weak point, provide a kind of method determining persimmon deastringent degree fast, this method is without special poisonous and harmful reagent, and reagent dosage is few, to human body and environmental pollution minimum, be eco-friendly method.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method determining persimmon deastringent degree fast, includes following steps:
(1) 5% ferric chloride solution is prepared: take 5.0g 5H
20FeCl
3in the ethanolic solution of 100ml 95%, add the hydrochloric acid that 1.0ml volume fraction is 34 ~ 36%, be stirred to 5H gently with glass bar
20FeCl
3dissolve completely, be stored in brown drop bottle for subsequent use.
(2) fruit is cut: the persimmon fruit processed taking away the puckery taste, along ambitus crosscut, notices that tangent plane keeps smooth, evenly to dip solution.
(3) dip: the calyx and receptacle of a persimmon position pinching persimmon after crosscut with hand, persimmon fruit tangent plane is immersed in the ferric chloride solution solution of first step preparation, continued for 10 ~ 15 seconds.
(4) colour developing is left standstill: persimmon fruit immersion liquid completed is taken out, left at room temperature 1 ~ 2 minute.
(5) adopt Forint phenol method to measure the soluble tannin content of the persimmon fruit of different colour developing degree, according to tannin content and colour developing degree, make the colour developing degree of specific persimmon kind and the standard control collection of illustrative plates of tannin content.
(6) degree of taking away the puckery taste is judged: according to colour developing depth degree, contrast the development criteria collection of illustrative plates of this kind, the degree of taking away the puckery taste of persimmon fruit can be judged immediately.
Tannin is extremely sensitive to metal ion, and its effect comprises two aspects, and one is electrostatic interaction, is physical process, namely by the dehydration of inorganic salts and the precipitation of saltout promotion tanning solution or colloid; Two is complex reactions, mainly chemical process, tannin forms five-membered ring with ortho position two phenolic hydroxyl group and metal ion, huge legendary turtle is closed in tannin molecule a lot of ortho positions phenolic hydroxyl group, can be used as polyhydroxy part and metal ion carries out ligand exchange reaction, the netted huge legendary turtle compound formed can precipitate at various ph values, and such as, tannin cell can be combined with iron ion and form black-and-blue deposit.
Add a small amount of hydrochloric acid in ferric chloride solution, can Fe be made
3+keep stable in acid condition.
During the present invention determines and is applicable to producing on the basis of test, puckery persimmon takes away the puckery taste the suitable decision method of degree, find out from result of the test, the how many and degree of taking away the puckery taste of tannin content can be judged in persimmon fruit fast, simple to operate, with low cost, to place equipment etc. without particular/special requirement, realistic production requirement.
The judgement that the present invention works out is taken away the puckery taste the method for degree, and without special poisonous and harmful reagent, and reagent dosage is few, to human body and environmental pollution minimum, be eco-friendly method.
Accompanying drawing explanation
Figure 1 shows that " gold urn persimmon " degree of taking away the puckery taste standard control collection of illustrative plates, in figure
I grade: very puckery, soluble tannin content 50 ~ 70%,
II grade: puckery, soluble tannin content 30 ~ 50%,
III grade: more puckery, soluble tannin content 10 ~ 30%,
IV grade: not puckery, soluble tannin content < 10%;
Figure 2 shows that " Mopan Persimmon " takes away the puckery taste degree standard control collection of illustrative plates, in figure
I grade: very puckery, soluble tannin content 50 ~ 70%,
II grade: puckery, soluble tannin content 30 ~ 50%,
III grade: more puckery, soluble tannin content 10 ~ 30%,
IV grade: not puckery, soluble tannin content < 10%;
Figure 3 shows that " headstock persimmon " degree of taking away the puckery taste standard control collection of illustrative plates, in figure
I grade: very puckery, soluble tannin content 50 ~ 70%,
II grade: puckery, soluble tannin content 30 ~ 50%,
III grade: more puckery, soluble tannin content 10 ~ 30%,
IV grade: not puckery, soluble tannin content < 10%;
Figure 4 shows that 95% Ethanol Treatment gold urn persimmon visual comparison after 24 hours;
Figure 5 shows that 95% Ethanol Treatment gold urn persimmon visual comparison after 48 hours;
Figure 6 shows that 95% Ethanol Treatment gold urn persimmon visual comparison after 72 hours;
Figure 7 shows that 95% Ethanol Treatment gold urn persimmon visual comparison after 96 hours;
Figure 8 shows that 95% ethanol postincubation Mopan Persimmon visual comparison after 24 hours;
Figure 9 shows that 95% ethanol postincubation Mopan Persimmon visual comparison after 48 hours;
Figure 10 shows that 95% ethanol postincubation Mopan Persimmon visual comparison after 72 hours;
Figure 11 shows that 95% ethanol postincubation Mopan Persimmon visual comparison after 96 hours;
Figure 12 shows that 95% ethanol postincubation headstock persimmon visual comparison after 24 hours;
Figure 13 shows that 95% ethanol postincubation headstock persimmon visual comparison after 48 hours;
Figure 14 shows that 95% ethanol postincubation headstock persimmon visual comparison after 72 hours;
Figure 15 shows that 95% ethanol postincubation headstock persimmon visual comparison after 96 hours.
Detailed description of the invention
Describe the present invention below in conjunction with the drawings and specific embodiments:
As shown be specific embodiments of the invention;
embodiment 1
Puckery persimmon kind " gold urn persimmon "
One, puckery persimmon takes away the puckery taste deciding degree method
Preparation ferric chloride solution → ethanol take away the puckery taste → cutting persimmon fruit → dip → leave standstill colour developing → judgement take away the puckery taste degree → with Forint phenol method comparative test result
According to said determination method, specifically comprise the following steps:
1) ferric chloride solution of 5% is prepared: take 5.0g 5H
20FeCl
3in the ethanolic solution of 100ml 95%, slowly add 1.0ml(volume fraction 35.4%) hydrochloric acid, be stirred to 5H gently with glass bar
20FeCl
3dissolve completely, be stored in brown drop bottle for subsequent use.
2) ethanol takes away the puckery taste: persimmon fruit is put into gas account, and spraying mass concentration to persimmon surface with the form of spraying is the ethanol of 95%, and then blanket gas account immediately, places at normal temperatures; Establish room temperature control (CK) simultaneously, namely naturally place without Ethanol Treatment room temperature.Once, get 10 fruits every 24 hours (hr) sampling during taking away the puckery taste at every turn.
3) cutting persimmon fruit: by persimmon fruit along ambitus crosscut, notices that tangent plane keeps smooth, evenly to dip solution.
4) dip: ferric chloride solution is poured in culture dish, pinch calyx and receptacle of a persimmon position with hand and persimmon fruit cross section is immersed in solution completely, continued for 12 seconds.
5) colour developing is left standstill: taken out by persimmon fruit, left at room temperature 1 minute.
6) degree of taking away the puckery taste is judged: colour developing result contrasts with Fig. 1 " gold urn persimmon " the degree standard diagram of taking away the puckery taste, find that the fruit surface colour development depth degree taken away the puckery taste 24 hours is corresponding with I grade of standard diagram, the 48 little fruit in season surface colour developments that take away the puckery taste are consistent with II grade, take away the puckery taste 72 little fruit in season surface colour developments and III grade basically identical, take away the puckery taste 96 hours consistent with IV.
7) Forint phenol method is adopted to measure soluble tannin content in persimmon fruit, contrast result of determination.
The present invention is preferred, and add a small amount of hydrochloric acid in described ferric chloride solution, object makes Fe
3+keep stable in acid condition.The present invention is preferred, the concrete operations that described Forint phenol method measures soluble tannin content are: get 5.0g persimmon pulp in persimmon ambitus, be cut into thin splinter and put into mortar, add 20.0ml 80% methanol solution to grind, centrifugal 10 minutes of 5000g, get supernatant, residue is cleaned again with the methanol solution of 20.0ml 80%, repeat above step, finally get supernatant and be settled to 50.0ml, then distilled water diluting 10 times is used, 1.0ml sample is got during mensuration, add 7.5ml distilled water, 0.5ml phenols reagent, after 3 minutes, add 1.0ml saturated sodium carbonate, under 725nm, absorbance is measured after lh, by tannic acid calibration curve being found corresponding tannin content.
Two, measurement result
Table 1 " gold urn persimmon " soluble tannin changes of contents (%)
Process |
0h |
24h |
48h |
72h |
96h |
CK group |
1.70 |
1.56 |
1.49 |
1.45 |
1.25 |
Ethanol treatment groups |
1.70 |
1.18 |
0.562 |
0.193 |
0.137 |
As seen from Table 1, period CK group of taking away the puckery taste soluble tannin changes of contents is little, and after room temperature places 96 hours, soluble tannin content only have dropped 26.5%; And ethanol treatment groups soluble tannin content declines very fast, after 96 hours, soluble tannin content have dropped 91.2%.
Iron chloride visual comparison during what Fig. 4 ~ 7 were reflected be Ethanol Treatment, as can be seen from Figure, during process, control group fruit face all presents black-and-blue, and depth degree is basically identical, and colour developing in 96 hours is not obvious with the depth difference that develops the color for 0 hour; Ethanol treatment groups fruit face look shoals gradually, Ethanol Treatment 96 hours consequence faces and 0 hour color distinction more obvious.In overall colour developing result and table 1 persimmon fruit, soluble tannin changes of contents trend is consistent, and this method is suitable for gold urn persimmon degree of taking away the puckery taste and judges fast as seen.
embodiment 2
With the main cultivation in Shandong Province puckery persimmon kind " mill " persimmon for examination material carries out taking away the puckery taste deciding degree.
One, puckery persimmon takes away the puckery taste deciding degree method
Preparation ferric chloride solution → ethanol take away the puckery taste → cutting persimmon fruit → dip → leave standstill colour developing → judgement take away the puckery taste degree → with Forint phenol method comparative test result
According to said determination method, specifically comprise the following steps:
1) ferric chloride solution of 5% is prepared: take 5.0g 5H
20FeCl
3in the ethanolic solution of 100ml 95%, slowly add 1.0ml(volume fraction 36.2%) hydrochloric acid, be stirred to 5H gently with glass bar
20FeCl
3dissolve completely, be stored in brown drop bottle for subsequent use.
2) ethanol takes away the puckery taste: persimmon fruit is put into gas account, and spraying mass concentration to persimmon surface with the form of spraying is the ethanol of 95%, and then blanket gas account immediately, places at normal temperatures; Establish room temperature control (CK) simultaneously, namely naturally place without Ethanol Treatment room temperature.Once, get 10 fruits every 24 hours (hr) sampling during taking away the puckery taste at every turn.
3) cutting persimmon fruit: by persimmon fruit along ambitus crosscut, notices that tangent plane keeps smooth, evenly to dip solution.
4) dip: ferric chloride solution is poured in culture dish, pinch calyx and receptacle of a persimmon position with hand and persimmon fruit cross section is immersed in solution completely, continued for 15 seconds.
5) colour developing is left standstill: taken out by persimmon fruit, left at room temperature 1 minute.
6) degree of taking away the puckery taste is judged: the result that will develop the color and Fig. 2 " Mopan Persimmon " the degree standard diagram of taking away the puckery taste contrast, find that I grade of fruit face look of fruit surface colour development depth degree and the standard diagram taken away the puckery taste 24 hours is corresponding, the 48 little fruit in season surface colour developments that take away the puckery taste are corresponding with II grade, take away the puckery taste 72 little fruit in season surface colour developments and III grade is consistent, take away the puckery taste 96 hours consistent with IV.
7) Forint phenol method is adopted to measure soluble tannin content in persimmon fruit, comparative test result.
The present invention is preferred, and add a small amount of hydrochloric acid in described ferric chloride solution, object makes Fe
3+keep stable in acid condition.The present invention is preferred, the concrete operations that described Forint phenol method measures soluble tannin content are: get 5.0g persimmon pulp in persimmon ambitus, be cut into thin splinter and put into mortar, add 20.0ml 80% methanol solution to grind, centrifugal 10 minutes of 5000g, get supernatant, residue is cleaned again with the methanol solution of 20.0ml 80%, repeat above step, finally get supernatant and be settled to 50.0ml, then distilled water diluting 10 times is used, 1.0ml sample is got during mensuration, add 7.5ml distilled water, 0.5ml phenols reagent, after 3 minutes, add 1.0ml saturated sodium carbonate, under 725nm, absorbance is measured after lhr, by tannic acid calibration curve being found corresponding tannin content.
Two, measurement result
Table 2 " Mopan Persimmon " soluble tannin changes of contents (%)
Mopan Persimmon |
0hr |
24hr |
48hr |
72hr |
96hr |
CK group |
1.13 |
0.992 |
0.894 |
0.741 |
0.689 |
Ethanol postincubation group |
1.13 |
0.785 |
0.420 |
0.237 |
0.106 |
Period CK group of taking away the puckery taste as shown in Table 2 soluble tannin changes of contents is little, and after room temperature places 96 hours, soluble tannin content only have dropped 39.0%; And ethanol treatment groups soluble tannin content declines very fast, Ethanol Treatment is after 96 hours, and soluble tannin content have dropped 90.6%.
Visual comparison's result of iron chloride during what Fig. 8 ~ 11 were reflected be Ethanol Treatment, as can be seen from Figure, during process, control group fruit surface colour development depth degree is little to time variations, and colour developing in 96 hours is not obvious with the depth difference that develops the color for 0 hour; Ethanol treatment groups fruit face look obviously shoals gradually.In overall colour developing result and table 2 persimmon fruit, soluble tannin changes of contents trend is consistent, and this method is suitable for Mopan Persimmon and takes away the puckery taste the quick judgement of degree as seen.
embodiment 3
One, puckery persimmon takes away the puckery taste deciding degree method
Preparation ferric chloride solution → ethanol take away the puckery taste → cutting persimmon fruit → dip → leave standstill colour developing → judgement take away the puckery taste degree → with Forint phenol method comparative test result
According to said determination method, specifically comprise the following steps:
1) ferric chloride solution of 5% is prepared: take 5.0g 5 hours
20FeCl
3in the ethanolic solution of 100ml 95%, slowly add 1.0ml(volume fraction 35.4%) hydrochloric acid, be stirred to 5 hours gently with glass bar
20FeCl
3dissolve completely, be stored in brown drop bottle for subsequent use.
2) ethanol takes away the puckery taste: persimmon fruit is put into gas account, and spraying mass concentration to persimmon surface with the form of spraying is the ethanol of 95%, and then blanket gas account immediately, places at normal temperatures; Establish room temperature control (CK) simultaneously, namely naturally place without Ethanol Treatment room temperature.Once, get 10 fruits every 24 hours (hr) sampling during taking away the puckery taste at every turn.
3) cutting persimmon fruit: by persimmon fruit along ambitus crosscut, notices that tangent plane keeps smooth, evenly to dip solution.
4) dip: ferric chloride solution is poured in culture dish, pinch calyx and receptacle of a persimmon position with hand and persimmon fruit cross section is immersed in solution completely, continued for 10 seconds.
5) colour developing is left standstill: taken out by persimmon fruit, left at room temperature 2 minutes.
6) degree of taking away the puckery taste is judged: colour developing result and Fig. 3 " headstock persimmon " the degree standard diagram of taking away the puckery taste contrast, find that the fruit surface colour development depth degree taken away the puckery taste 24 hours is corresponding with I grade of standard diagram, the 48 little fruit in season surface colour developments that take away the puckery taste correspond to II grade, the 72 little fruit in season surface colour developments that take away the puckery taste are consistent with III grade, take away the puckery taste 96 hours consistent with IV.
7) Forint phenol method is adopted to measure soluble tannin content in persimmon fruit, contrast result of determination.
The present invention is preferred, and add a small amount of hydrochloric acid in described ferric chloride solution, object makes Fe
3+keep stable in acid condition.The present invention is preferred, the concrete operations that described Forint phenol method measures soluble tannin content are: get 5.0g persimmon pulp in persimmon ambitus, be cut into thin splinter and put into mortar, add 20.0ml 80% methanol solution to grind, centrifugal 10 minutes of 5000g, get supernatant, residue is cleaned again with the methanol solution of 20.0ml 80%, repeat above step, finally get supernatant and be settled to 50.0ml, then distilled water diluting 10 times is used, 1.0ml sample is got during mensuration, add 7.5ml distilled water, 0.5ml phenols reagent, after 3 minutes, add 1.0ml saturated sodium carbonate, under 725nm, absorbance is measured after l hour, by tannic acid calibration curve being found corresponding tannin content.
Two, measurement result
Table 3 " headstock persimmon " soluble tannin changes of contents (%)
Headstock persimmon |
0 hr |
24hr |
48hr |
72hr |
96hr |
CK group |
1.33 |
1.17 |
1.08 |
0.924 |
0.795 |
95% ethanol postincubation group |
1.33 |
0.932 |
0.616 |
0.309 |
0.127 |
As seen from Table 3, during taking away the puckery taste, control group soluble tannin content declines to some extent, and after room temperature places 96 hours, soluble tannin content reduces 40.2%; Ethanol treatment groups soluble tannin content declines very fast, and Ethanol Treatment is after 96 hours, and soluble tannin content have dropped 82.9%.
Can be found out by Figure 12 ~ 15, during process, control group fruit face all presents black-and-blue, and colour developing degree changes not quite in time; Ethanol treatment groups fruit face look shoals gradually, and Ethanol Treatment is shallow when after 96 hours, color is obviously little than 0.In overall colour developing result and table 3 persimmon fruit, soluble tannin changes of contents trend is consistent, and this method is suitable for headstock persimmon degree of taking away the puckery taste and judges fast as seen.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited in above-mentioned citing, and the change that those skilled in the art make in essential scope of the present invention, remodeling, interpolation or replacement also should belong to protection scope of the present invention.