CN102523781A - Preparation method of dual fluorescence anti-counterfeiting pelletized seed and test method thereof - Google Patents
Preparation method of dual fluorescence anti-counterfeiting pelletized seed and test method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of dual fluorescence anti-counterfeiting pelletized seed, comprising the following steps of: firstly applying a solution of a first fluorescent colorant on naked seed in a spraying way, coating a first seed coating agent, applying adhesive in a spraying way, coating a layer of the first seed coating agent, mixing a second seed coating agent with powder of a second fluorescent colorant with a certain quantity, and coating the pelletized seed. The invention further provides a test method of the pelletized seed and early seedlings formed by cracking under the irradiation of the exciting light with two wavelengths. The invention has the advantage that the anti-counterfeiting cost is low since the method is simply adjusted on the basis that the original pelletization process flow of the tobacco seed is not changed, and the equipment does not need updating. Compared with the common tobacco pelletized seed, the tobacco pelletized seed with double-fluorescent anti-counterfeiting function has the same appearance, and only can show fluorescent characteristic only under specific detection step and detection light. The method provides a more perfect anti-counterfeit technology for the seed industry.
Description
Background technology
The present invention relates to anti-counterfeiting technology, be specifically related to the preparation method of the false proof pelleted seed of a kind of double fluorescent, also relate to the discrimination method of the false proof seed of this method acquisition.
Technical field
Seed occupies critical role in national economy, but seed often faces the situation of being palmed off by the lawless person, and this brings very big harm for agricultural production and peasant.False proof about seed, what industry was generally used at present all is the anti-counterfeit package technology.Seed packaging is the direct carrier that seed is sold, so fake and forged, as to safeguard seed market normal order, protection number one and legitimate rights and interests comparatively direct, effective solution are hit by the false proof seed enterprise that also becomes naturally of seed packaging.But mixing the genuine with the fictitious and the confusion of anti-fake product itself of packaging industry makes that seed enterprise is hard to guard against, also lets ordinary people hard to tell whether it is true or false.And to also less the appearing in the newspapers of anti-counterfeiting technology of seed itself.
Seed-pelleting has been kind of the technology of industry widespread usage, especially granule and minimum grain seed at present, and its pill processing technology reaches its maturity, also mostly adopts its pill pelleting seed to sow in the production.
About the anti-counterfeiting technology of seed, Chinese patent CN101403694A discloses a kind of fluorescence falsification preventing and detection method that is used for capsuled seed.Comprise the steps: 1) toner of the shinny yellow fluorescence of a kind of ultraviolet is joined in the solvent, concentration is 0.5～3mg/ml, and agitator speed is transferred to 400～600 rev/mins, stirs until becoming uniform solution, solvent is a pH value at 7.2～8.0 phosphate buffer; Used clear water when 2) step 1) gained solution being substituted the seed internal layer coating repeatedly sprays when internal layer coating; 3) other technological processes of seed pelleting are constant.
Chinese patent CN101971727A discloses a kind of preparation and discriminating conduct with anti-fraud functional capsuled seed.This method is that fluorescence toner and solvent are processed certain density homogeneous fluorescence solution according to described technology, when internal layer pulvis dressing, sprays with fluorescence solution then, carries out seed pelleting by conventional method and handles, and obtains having anti-fraud functional capsuled seed.It is fluorescein that this patent application further discloses the fluorescence toner that adopts.
Fluorescein is the fluorescence toner of non-toxic and safe.Fluorescein also has report proof fluorescein can improve the growth performance of plant root on plant by extensive utilization aspect the health detection of medical science and animal, promotes growth and development of plant.And the growth of plant originates from seed, has facilitation itself just to explain that fluorescein is nonhazardous to seed to plant growing.Simultaneously; Seed vitality is the important indicator of seed quality; Certain compound is to the evaluation of seed vitality impact effect; Usually judge according to seed sprouting and growth of seedling situation, the height of seed vitality is described through measuring indexs such as seed germination rate, germination vigor, germination index and seedling root length, height of seedling after planting.Fluorescein can improve the growth performance of plant root, promotes growth and development of plant, explains that thus it also has facilitation to the germination of seed and the growth and the growth of the whole seedling of plant phase of seedling root.
But it is single false proof that existing fluorescence falsification preventing method belongs to, and its shortcoming is when carrying out seed-pelleting, only to have added a kind of fluorescent material; Detection method is single; False proof safety is lower, and can only when the seed cracking, carry out anti-counterfeiting detection, can't carry out false proof to seedling.
And the present invention is exactly the problem that exists to the single fluorescence falsification preventing method of pelleted seed; Combine with pillization fluorescent dual is false proof; And two kinds of different fluorescent materials are applied in the seed-pelleting process, when guaranteeing that fluorescent material and processing mode are to seed sprouting and growth of seedling nonhazardous effect, can avoid the false proof lower defective of expensive and single anti-forgery security of packaging material again to greatest extent; Simultaneously, in the false proof effect of seedling stage also tool.
Summary of the invention
An object of the present invention is to provide the preparation method of the false proof pelleted seed of a kind of double fluorescent, under the situation that guarantees seed activity, solved the fake and forged problem of seed on the market.The easy easy operating of this method for anti-counterfeit, false proof cost is low, and the antiforge function of pelleted seed is strengthened, thereby has protected the interests of wide farmers and seeds company greatly.
The preparation method of the false proof pelleted seed of a kind of double fluorescent comprises the steps:
1, granulation: pour the naked kind of certain mass into the dressing machine, the naked kind of the solution wetted of the first fluorescence toner of spraying preparation surface, adding quality is first kind of clothing agent of the naked mass of 3.5%-5.0%; Constantly stir; Make it to be wrapped in naked kind surface, repeat above step 3-5 time, form little pellets; First kind of clothing agent and the repeat number time that add the naked mass of 20%-50% then at every turn, during continuous spray adhesive and stirring;
2, Pelleting: obtain mixture after doubly the pulvis of the second fluorescence toner of second kind of clothing agent and the naked mass of 5%-15% of naked mass mixes with 7-43; The ball shape seed that the mixture that repeatedly adds naked mass 20%-50% then formed to last step, during continuous spray adhesive and stirring, screen then, polish, paint, drying, obtain the seed that dressing finishes.
Wherein, the described first fluorescence toner is a rhodamine B, and the described second fluorescence toner is a fluorescein.
Wherein, the agent of kind clothing is optional from clay, diatomite, peat, mica, vermiculite, the mixing of one or more in perlite, active carbon, rock phosphate, bentonite and the talcum powder.Described first kind of clothing agent is selected from bentonite.Described second kind of clothing agent is selected from talcum powder.Described adhesive is to be selected from the solution that high molecular polymer forms; High molecular polymer comprises gum Arabic; Starch, carboxymethyl cellulose, methylcellulose; Ethyl cellulose, polyethylene acetate fiber (salt), Sodium Alginate, polyvinylidene chloride, polyethylene oxide, polyvinyl alcohol etc., preferably carboxymethyl cellulose.The aqueous solution of described adhesive preferably carboxymethyl cellulose, its concentration are 0.5%-3% (percentage by weight).
Wherein, Described seed is plant seeds such as the vegetables that are fit to Pelleting, flowers, herbage, economic crops, vegetable seeds such as cauliflower, wild cabbage, rape etc., flower seed such as Malus spectabilis, petunia etc.; Grass seed such as alfalfa, lyme grass etc., economic crops such as tobacco, sesame etc.
Wherein, said seed is preferably the seed that in actual production, needs through pill processing granule and minimum grain, and further preferred thousand kernel weight is less than the seed of 5g, and preferred especially thousand kernel weight is at the minimum grain seed of 0.05-0.5g.
Wherein, in granulation step, the gross mass that adds the first fluorescence toner is preferably the 0.45%-0.75% of naked mass.
Wherein, in the Pelleting step, the gross mass that adds the second fluorescence toner is preferably 5% or 10% or 15% of naked mass, and most preferably 10%.
Wherein, plant the period of the day from 11 p.m. to 1 a.m at the minimum grain of 0.05-0.5g when seed is a thousand kernel weight, the 6-9 that the first kind of clothing agent quality that in granulation step, adds adds up to naked mass doubly, preferred 7.5 times.
Wherein, plant the period of the day from 11 p.m. to 1 a.m at the minimum grain of 0.05-0.5g when seed is a thousand kernel weight, the 35-43 that the second kind of clothing agent quality that in the Pelleting step, adds adds up to naked mass doubly, preferred 42 times.
Wherein, when granulation step finished, the particle diameter of minimum grain pelleted seed was 1.00mm-1.25mm, and when the Pelleting step finished, the particle diameter of minimum grain pelleted seed was 1.60mm-1.80mm.
The present invention also provides a kind of double fluorescent false proof seed; Wherein, With naked kind is that core is coated with three-decker; The ground floor structure of wrapping up naked kind comprises the first kind of clothing agent and the first fluorescence toner, and the second layer structure of parcel ground floor structure comprises first kind of clothing agent, and the three-decker of parcel second layer structure comprises the second kind of clothing agent and the second fluorescence toner.
Wherein, the described first fluorescence toner is a rhodamine B, and the described second fluorescence toner is a fluorescein.
Wherein, the agent of kind clothing is optional from clay, diatomite, peat, mica, vermiculite, the mixing of one or more in perlite, active carbon, rock phosphate, bentonite and the talcum powder.Described first kind of clothing agent is selected from bentonite.Described second kind of clothing agent is selected from talcum powder.Described adhesive is to be selected from the solution that high molecular polymer forms; High molecular polymer comprises gum Arabic; Starch, carboxymethyl cellulose, methylcellulose; Ethyl cellulose, polyethylene acetate fiber (salt), Sodium Alginate, polyvinylidene chloride, polyethylene oxide, polyvinyl alcohol etc., preferably carboxymethyl cellulose solution.The aqueous solution of described adhesive preferably carboxymethyl cellulose, its concentration are 0.5%-3% (percentage by weight).
Wherein, in the said ground floor structure, the content of the first fluorescence toner is the 0.45%-0.75% of naked mass.
Wherein, in the said three-decker, the content of the second fluorescence toner is the 5%-15% of naked mass, preferred 5% or 10% or 15%, most preferably 10%.
Wherein, plant the period of the day from 11 p.m. to 1 a.m at the minimum grain of 0.05-0.5g when seed is a thousand kernel weight, the 6-9 that said first kind of clothing agent quality adds up to naked mass doubly, preferred 7.5 times.
Wherein, plant the period of the day from 11 p.m. to 1 a.m at the minimum grain of 0.05-0.5g when seed is a thousand kernel weight, the 35-43 that said second kind of clothing agent quality adds up to naked mass doubly, preferred 42 times.
Wherein, plant the period of the day from 11 p.m. to 1 a.m when seed is a thousand kernel weight at the minimum grain of 0.05-0.5g, when granulation step finished, the particle diameter of pelleted seed was 1.00mm-1.25mm, and when the Pelleting step finished, the particle diameter of pelleted seed was 1.60mm-1.80mm.
Another purpose of the present invention provides the method for the false proof seed of a kind of fast detecting double fluorescent, and this method comprises the steps:
At first pelleted seed is placed on the slide; Add water and make its cracking; The pelleted seed that adds water-splitting with the blue light illumination of wave-length coverage 480nm～500nm; Then shine the pelleted seed of cracking then with the green glow of wave-length coverage 520nm～540nm as if the inner green fluorescence that becomes clear that shows of pelleted seed under irradiation, if the red fluorescence that the inner demonstration of pelleted seed becomes clear under irradiation, then described pelleted seed is the false proof seed of double fluorescent.
The present invention also provides the method for the false proof seed of a kind of fast detecting double fluorescent, and this method comprises the steps:
Pelleted seed is sprouted; With the early stage seedling of the blue light illumination of wave-length coverage 480nm～500nm; If seedling can show bright yellow-green fluorescence under irradiation; Then then with the green glow irradiation of wave-length coverage 520nm～540nm, if seedling shows bright red fluorescence under irradiation, then described pelleted seed is the false proof seed of double fluorescent.
Wherein, The tobacco pelleted seed is sprouted; With two cotyledons of the early stage seedling of the blue light illumination of wave-length coverage 480nm～500nm,, then shine with the green glow of wave-length coverage 520nm～540nm then if show bright yellow-green fluorescence with the stem growing point in that cotyledon is most advanced and sophisticated; If the cotyledon vein shows bright red fluorescence under irradiation, then described pelleted seed is the false proof seed of double fluorescent.
Wherein, do not have the branch of strict priority with blue light illumination with the step of green glow irradiation.
The invention has the advantages that: simple to operation, on the basis that does not change the original Pelleting technological process of seed, simply adjust, need not the renewal of equipment etc., with low cost.This have the anti-fraud functional pelleted seed of a double fluorescent and common pelleted seed indifference in appearance, only under specific detection step and the irradiation that detects light, just can demonstrate the double fluorescent characteristic.And because detect anti-fake mark in the seedling in early days, therefore, can get the field seedling and detect, distinguish the true from the false, improve false proof ageing largely if peasant household implements after planting to go wrong.This method has guaranteed the quality of seed for the seed industry provides more perfect anti-counterfeiting technology, has protected seed enterprise and the interests of planting child user.
Description of drawings
Fig. 1 is the fluorescence performance during the false proof pelleted seed cracking of double fluorescent among the embodiment 2;
Fig. 2 is that the false proof pelleted seed of double fluorescent germinateed the 7th day and the fluorescence performance of the 16th day seedling among the embodiment 2;
Fluorescence performance when Fig. 3 is the pelleted seed cracking after fluorescein is handled among the embodiment 3;
Fig. 4 is the germinate fluorescence performance of the 7th day seedling of the pelleted seed after fluorescein is handled among the embodiment 3.
Embodiment
Provide preferred embodiment of the present invention below, these embodiment and unrestricted content of the present invention.
Among the following embodiment, the seed of tobacco bred " MS cloud and mist 85 " and " the big gold dollar of safflower " is from China Tobacco Seed Yuxi Co., Ltd.." MS cloud and mist 85 " thousand grain weigth is 0.085g, and " the big gold dollar of safflower " thousand grain weigth is 0.081g.Rape seed is available from Hangzhou, Zhejiang province city seeds company, and alfalfa seed is available from Zhejiang Hangzhou grass seed company.Bentonite and talcum powder are from China Tobacco Seed Yuxi Co., Ltd., and carboxymethyl cellulose is available from Hangzhou Huadong Medicine Group Co.,Ltd.The model of dressing machine is BY300A, available from the new promise instrument and equipment in Shanghai Co., Ltd.Rhodamine B and fluorescein are from Advtechind Corporation.
Embodiment 1The preparation method of the false proof tobacco pelleted seed of double fluorescent
Pour 10g " MS cloud and mist 85 " tobacco seed into the dressing machine.
Granulation: get the 200mg rhodamine B and add that preparation concentration is the rhodamine B aqueous solution of 2.0mg/ml in the distilled water; The moistening the surface of the seed of the rhodamine B aqueous solution of the spraying 7.5ml of elder generation; Constantly stir after adding quality and be the bentonite of 0.5g; Make it be wrapped in the surface of the seed, repeat above-mentioned steps 3-5 time, make seed form little pellets; The 2-5g bentonite is joined in the ball shape seed then, spraying concentration is 1.0% cmc soln, constantly stirs, and repeats repeatedly, makes the particle diameter of ball shape seed be increased to 1.00mm-1.25mm at every turn;
Pelleting: 1g fluorescein pulvis and 420g talcum powder are mixed; The 2-5g mixture is joined in the ball shape seed of granulation formation; The cmc soln of spraying 2.0% constantly stirs, and repeats repeatedly; Make the particle diameter of the ball shape seed that granulation forms be increased to 1.60mm-1.80mm, screen then, polish, paint, drying obtains the seed that dressing finishes.
When granulation step begins, at first add a small amount of clothing agent of planting, can make that seed fully disperses, help the later stage granulation, the purpose of granulation is that seed is further disperseed and increases its volume, Pelleting then makes the seed volume after the granulation continue to increase to ideal range.The control of pelleted seed particle diameter is mainly screened through the sifting machine of difformity with size, and the seed that reaches desirable particle size sifts out, the then continuation Pelleting that does not reach.
Because rhodamine B is water-soluble fine, and fluorescein is water-soluble relatively poor, is reducing cost as far as possible, simplify preparation process, can reach again under the prerequisite of effective fluorescence falsification preventing, the suitable treatment method that filters out rhodamine B and fluorescein is measured with handling.Replace clear water to add the ground floor structure to rhodamine B fluorescence solution simultaneously; Second layer structure is not added any fluorescent material; Three-decker is added fluorescein again, and the one, for fear of the mixing colour contamination of two kinds of fluorescence toners, the 2nd, in order to increase false proof identifiability.
It is optional from clay, diatomite to plant the clothing agent, peat, mica, vermiculite, the mixing of one or more in perlite, active carbon, rock phosphate, bentonite and the talcum powder.First kind of clothing agent in the present embodiment is preferably from bentonite.Second kind of clothing agent is preferably from talcum powder.Its main cause is that these two kinds of raw material chemical property are stable, composition is single, cheap and easy to get, be easy to suitability for industrialized production.
Described adhesive is to be selected from the solution that high molecular polymer forms; High molecular polymer comprises gum Arabic; Starch, carboxymethyl cellulose, methylcellulose; Ethyl cellulose, polyethylene acetate fiber (salt), Sodium Alginate, polyvinylidene chloride, polyethylene oxide, polyvinyl alcohol etc., present embodiment preferably carboxymethyl cellulose solution.The aqueous solution of described adhesive preferably carboxymethyl cellulose, its concentration are 0.5%-3% (percentage by weight).
Simultaneously, get " the big gold dollar of safflower " seed 10g,, obtain the big gold dollar pelleted seed of safflower finished product through aforesaid pill operation.
In addition; The contrast pelleted seed for preparing a certain amount of MS cloud and mist 85 and the big gold dollar of safflower; Concrete preparation method is similar with preceding method; Its difference is, in granulation step, replaces rhodamine B solution to spray with distilled water, in the Pelleting step, does not add the fluorescein pulvis and prepares pelleted seed.Contrast is all represented with CK.
Pelleted seed germinates and the seedling physiology index is measured to handling and contrasting with following method.
(1) seed sprouting and seedling index
Pelleted seed is placed the diameter 9cm culture dish of three layers of moisture absorption filter paper.Every processing repeats 100 pelleted seeds of every repetition 3 times.The experiment of germinateing is carried out under 20～30 ℃ of alternating temperature conditions, high temperature (30 ℃) 8h, and low temperature (20 ℃) 16h, the high temperature period has illumination.
Put bed back and played every day on the 2nd day germination seed is counted, calculated germination vigor in the 7th day, the 16th day statistics germination rate.Germinateed the 17th day, 3 of each processing are repeated all to select 10 strain seedling at random, measure the long and height of seedling of its root.Seedling is dried 24h in 80 ℃ of baking ovens, measure its dry weight.Germination index (GI=∑ (G
t/ T
t)) (in the formula: G
tBe the germinative number of different time, T
tBe the germination fate, ∑ is a summation), vitality index (VI=GI * seedling dry weight).
(2) seedling chlorophyll content
Get the bright appearance of the seedling 0.2g of different disposal, place mortar, add 1ml 95% ethanol and grind, after fully grinding, pour in the 5ml centrifuge tube, add 2ml 95% alcohol flushing again, pour in the centrifuge tube, in the centrifugal 10min of 5000r/min.Get supernatant 1ml in the 10ml centrifuge tube, add 9ml 95% ethanol, measure 665 behind the mixing; 649, absorbance under the 470nm is a blank with 95% ethanol; The computational methods of chlorophyll a, chlorophyll b, carotenoid and chlorophyll total content are with reference to Li Hesheng; The method of definition in " plant physiology and biochemistry experimental principle and the technology " that Sun Qun, Zhao Shijie etc. write (Beijing: Higher Education Publishing House, 2001).
(3) seedling protective enzyme activity determination method:
Get the bright appearance of the seedling 0.5g after the different disposal; In the 0.05M of 10ml phosphate buffer (pH7.8), be ground to homogenate; With the centrifugal 15min of 10000r/min, get supernatant and carry out the protective enzyme determination of activity as enzyme extract then, institute all carries out under 4 ℃ of low temperature in steps.Catalase (CAT) determination of activity, the method for pressing Cao etc. (2010), changing 0.01 with per minute A240 is 1 unit of enzyme activity; Guaiacol method (Qiu etc., 2005) is adopted in peroxidase (POD) determination of activity, and changing 0.01 with per minute A470 is 1 unit of enzyme activity; Superoxide dismutase (SOD) determination of activity is with reference to (2007) such as Zhang.
(4) statistical analysis technique
Adopt SAS (V8) software to carry out variance analysis, multiple ratio adopts P＜0.05, the LSD method, and the percentage data of result of the test transforms (y=arcsin [sqr (x/100)]) through arcsine earlier before the statistics.
Measure the result shown in following form:
The influence to seed sprouting and seedling quality is handled in the false proof Pelleting of table 1 double fluorescent
*The same kind different disposal of different letter representations differences significantly (P＜005, LSD), down with
The false proof Pelleting of table 2 double fluorescent is handled the active influence of seedling protective enzyme
The influence to chlorophyll content in the seedling is handled in the false proof Pelleting of table 3 double fluorescent
Can find out by measuring the result; Replace water to spray when the Pelleting of seed internal layer with certain density rhodamine B solution; Again encapsulate the kind clothing agent of having added fluorescein thereafter; The false proof processing of this double fluorescent all has no adverse effects to seed sprouting, growth of seedling, seedling protective enzyme activity, and has improved the chlorophyllous content of tobacco seedling to a certain extent.
Embodiment 2The detection method of the false proof tobacco pelleted seed of double fluorescent
The MS cloud and mist 85 double fluorescent pelleted seeds that embodiment 1 is prepared are placed on the slide; Add water and make its cracking; With the blue light illumination of wave-length coverage 480nm～500nm, find the inner green fluorescence that becomes clear that shows of pelleted seed, shine the pelleted seed of cracking then with the green glow of wave-length coverage 520nm～540nm; The inner red fluorescence that becomes clear that shows of discovery pelleted seed under irradiation explains that this pelleted seed is the false proof pelleted seed of double fluorescent.
MS cloud and mist 85 double fluorescent pelleted seeds are sprouted; With two cotyledons of the early stage seedling of the blue light illumination of wave-length coverage 480nm～500nm; Most advanced and sophisticated and the bright yellow-green fluorescence of stem growing point demonstration at cotyledon; Then with the green glow irradiation of wave-length coverage 520nm～540nm, the cotyledon vein shows bright red fluorescence, explains that this pelleted seed is the false proof pelleted seed of double fluorescent.
With the method for present embodiment seed being carried out the true and false detects; Find that pelleted seed is when the suction cracking; In the down no fluorescence performance of natural daylight; But can be observed tangible green fluorescence through blue-light excited at the cracking position, excite through green glow to can be observed red fluorescence, the contrast pelleted seed that does not add fluorescent material does not then have fluorescence performance (Fig. 1).The growth of seedling of the false proof processing of double fluorescent is in the time of the 7th day; In the down no fluorescence performance of natural daylight; But can be observed bright green fluorescence (Fig. 2 at blue-light excited seedling cotyledon tip down and stem growing point; A-a), and green glow excite down the seedling cotyledon vein can be observed tangible red fluorescence (Fig. 2, A-b).Growth of seedling is in the time of the 16th day, and two kinds of fluorescence are still visible, just brightness deterioration (Fig. 2, B-a and B-b).And the contrast seedling of not adding fluorescent material does not all have fluorescence performance (Fig. 2, CK-a and CK-b) under two kinds of exciting lights.
Fig. 1 is that the fluorescence under different exciting lights shows after the MS cloud and mist 85 double fluorescent pelleted seeds suctions cracking for preparing of embodiment 1, and blank light refers to natural daylight.The upper strata is not for adding the control group pelleted seed (CK) of fluorescent material, and ((no fluorescence shows under the irradiation of wave-length coverage 520nm～540nm) for wave-length coverage 480nm～500nm) and green glow at blue light.The double fluorescent pelleted seed of lower floor is at blue-light excited bright green fluorescence, the bright red fluorescence of demonstration under green glow excites of showing down.
Fig. 2 is the fluorescence performance that the false proof pelleted seed of MS cloud and mist 85 double fluorescents is sprouted the back seedling; Wherein CK representes not add the control group of fluorescent material; A represents the fluorescence performance of the false proof processing growth of seedling of double fluorescent in the time of the 7th day; B represents the fluorescence performance of the false proof processing growth of seedling of double fluorescent in the time of the 16th day; CK-a and CK-b represent not add the fluorescence performance of contrast seedling under blue light and green glow of fluorescent material respectively, and A-a and A-b represent the performance of the fluorescence under blue light and green glow in the time of the 7th day of the false proof processing growth of seedling of double fluorescent respectively, and B-a and B-b represent the performance of the fluorescence under blue light and green glow in the time of the 16th day of the false proof processing growth of seedling of double fluorescent respectively; This figure amplifies 20 times, and blank light promptly refers to natural daylight.
Embodiment 3The preparation method who possesses the tobacco pelleted seed of single fluorescence
For the ease of embodying the advantage of the present invention with respect to prior art, the tobacco pelleted seed that at present prepares a certain amount of single fluorescence compares.
At first with Na
2HPO
42H
2O 35.61g or Na
2HPO
47H
2O 53.65g or Na
2HPO
412H
2O 71.7g uses the 800ml dissolved in distilled water, and then is settled to 1000ml with distilled water, is mixed with 0.2mol/L Na
2HPO
4Solution, i.e. mother liquor A; With NaH
2PO
4H
2O 27.6g or NaH
2PO
42H
2O 31.2g uses the 800ml dissolved in distilled water, and then is settled to 1000ml with distilled water, is mixed with 0.2mol/L NaH
2PO
4Solution, i.e. mother liquor B; With mother liquor A (x ml) with after mother liquor B (y ml) mixes again with distilled water diluting to 200ml, obtain as shown in the tablely, concentration is 0.1mol/L, the phosphate buffer that the pH value is different:
| x(ml) | y(ml) | pH |
| 72.0 | 28.0 | 7.2 |
| 77.0 | 23.0 | 7.3 |
| 81.0 | 19.0 | 7.4 |
| 84.0 | 16.0 | 7.5 |
| 87.0 | 13.0 | 7.6 |
| 89.5 | 10.5 | 7.7 |
| 91.5 | 8.5 | 7.8 |
| 93.0 | 7.0 | 7.9 |
| 94.7 | 5.3 | 8.0 |
Next fluorescein pulvis joins in the phosphate buffer of above-mentioned steps preparation, stirs with agitator, and obtaining concentration is the fluorescence solution of 0.5～3mg/ml, and agitator speed is 400～600 rev/mins.
It is similar to possess the preparation method who provides among preparation method and the embodiment 1 of pelleted seed of single fluorescence; Its difference is; Fluorescence solution with the above-mentioned steps preparation in granulation step replaces rhodamine B solution to spray, and in the Pelleting step, does not add the fluorescein pulvis.
Fig. 3 be embodiment 3 prepare single fluorescence pelleted seed suction cracking the time fluorescence under the different wave length exciting light show, blank light promptly refers to natural daylight.The single fluorescence pelleted seed of right side one row only at the blue-light excited green fluorescence that becomes clear that shows down, excites down no fluorescence performance at green glow; When being listed as the control group pelleted seed suction cracking of not adding fluorescent material, left side one under two kinds of exciting lights irradiations, all do not have the fluorescence performance.
Fig. 4 is the fluorescence performance in the seedling that germinateed the 7th day of the pelleted seed after the single fluorescence of fluorescein is handled.Can see that the growth of seedling that single fluorescence is handled is in the time of the 7th day, through blue-light excited, seedling fluorescence has not had any difference with the contrast seedling of not adding fluorescent material.
This single false proof processing has following shortcoming with respect to the false proof processing of double fluorescent: the one, and fluorescein is not soluble in water, the formulations prepared from solutions complex operation; The 2nd, growth of seedling has not had the fluorescence performance in early days, and the fluorescence labeling continuation is poor; The 3rd, have only a kind of anti-fake mark, easy quilt is copied.
Embodiment 4The preparation method of the false proof rape pelleted seed of double fluorescent
Pour the rape seed of 10g into the dressing machine, its thousand kernel weight is 4.5g.
Granulation: get the 200mg rhodamine B and add that preparation concentration is the rhodamine B aqueous solution of 2.0mg/ml in the distilled water; The moistening the surface of the seed of the rhodamine B aqueous solution of the spraying 7.5ml of elder generation; Constantly stir after adding quality and be the bentonite of 0.5g; Make it be wrapped in the surface of the seed, repeat above-mentioned steps 3-5 time, make seed form little pellets; The 2-5g bentonite is joined in the ball shape seed then, spraying concentration is 0.5% cmc soln, constantly stirs, and repeats repeatedly, makes the particle diameter of ball shape seed be increased to 2.80mm-2.90mm at every turn;
Pelleting: 1.5g fluorescein pulvis and 70g talcum powder are mixed; The 2-5g mixture is joined in the ball shape seed of granulation formation at every turn; The cmc soln of spraying 1.0% constantly stirs, and repeats repeatedly; Make the particle diameter of the ball shape seed that granulation forms be increased to 3.00mm-3.20mm, screen then, polish, paint, drying obtains the seed that dressing finishes.
After the method that present embodiment provides was carried out the false proof Pelleting of double fluorescent and handled rape seed, seed can be observed tangible green fluorescence through blue-light excited at the cracking position when the suction cracking, and excited through green glow and can be observed red fluorescence.
The growth of seedling of the false proof processing of double fluorescent can be observed bright green fluorescence blue-light excited seedling down in the time of the 5th day, and seedling can be observed tangible red fluorescence and excite down at green glow.
Embodiment 5The preparation method of the false proof alfalfa pelleted seed of double fluorescent
Pour the alfalfa seed of 10g into the dressing machine, its thousand kernel weight is about 1.1g.
Granulation: get the 200mg rhodamine B and add that preparation concentration is the rhodamine B aqueous solution of 2.0mg/ml in the distilled water; The moistening the surface of the seed of the rhodamine B aqueous solution of the spraying 7.5ml of elder generation; Constantly stir after adding quality and be the bentonite of 0.35g; Make it be wrapped in the surface of the seed, repeat above-mentioned steps 3-5 time, make seed form little pellets; The 2-5g bentonite is joined in the ball shape seed then, spraying concentration is 1.0% cmc soln, constantly stirs, and repeats repeatedly, makes the particle diameter of ball shape seed be increased to 1.40mm-1.60mm at every turn;
Pelleting: 0.5g fluorescein pulvis and 250g talcum powder are mixed; The 2-5g mixture is joined in the ball shape seed of granulation formation at every turn; The cmc soln of spraying 3.0% constantly stirs, and repeats repeatedly; Make the particle diameter of the ball shape seed that granulation forms be increased to 1.80mm-2.00mm, screen then, polish, paint, drying obtains the seed that dressing finishes.
The method that present embodiment provides when seed suction cracking, can be observed tangible green fluorescence through blue-light excited at the cracking position after adopting the false proof Pelleting of double fluorescent to handle to alfalfa seed, and excites through green glow and can be observed red fluorescence.
The growth of seedling of the false proof processing of double fluorescent can be observed bright green fluorescence blue-light excited seedling down in the time of the 5th day, and seedling can be observed tangible red fluorescence and excite down at green glow.
It is considered herein that preferable double anti-forge handles and must possess two conditions, the one, seed germination and growth of seedling are had no adverse effects, the 2nd, pelleted seed suction cracking in addition in early days the privileged sites of seedling can detect two kinds of anti-fake marks simultaneously.Compare with single fluorescence falsification preventing method, double anti-forge is handled and has been improved false proof safety and reliability, is difficult to imitated.And the double fluorescent antifalse effect can extend to seed germination and grow up to (different seeds it sprout to forming the seedling fate different) in the seedling after some day; Increased false proof ageing, make not only can be false proof on seed also the seedling stage is distinguished the true and false of seed in early days.
Claims (10)
1. the preparation method of the false proof pelleted seed of double fluorescent comprises the steps:
Granulation: pour the naked kind of certain mass into the dressing machine, the naked kind of the solution wetted of the first fluorescence toner of spraying preparation surface, adding quality is first kind of clothing agent of the naked mass of 3.5%-5.0%; Constantly stir; Make it to be wrapped in naked kind surface, repeat above step 3-5 time, form little pellets; First kind of clothing agent and the repeat number time that add the naked mass of 20%-50% then at every turn, during continuous spray adhesive and stirring;
Pelleting: obtain mixture after doubly the pulvis of the second fluorescence toner of second kind of clothing agent and the naked mass of 5%-15% of naked mass mixes with 7-43; The ball shape seed that the mixture that repeatedly adds naked mass 20%-50% then formed to last step, during continuous spray adhesive and stirring, screen then, polish, paint, drying, obtain the seed that dressing finishes.
2. the preparation method of false proof seed as claimed in claim 1 is characterized in that, the described first fluorescence toner is a rhodamine B, and the described second fluorescence toner is a fluorescein.
3. the preparation method of false proof seed as claimed in claim 2 is characterized in that, the agent of kind clothing is optional from clay, diatomite, peat, mica, vermiculite, the mixing of one or more in perlite, active carbon, rock phosphate, bentonite and the talcum powder; Described first kind of clothing agent is selected from bentonite; Described second kind of clothing agent is selected from talcum powder; Described adhesive is to be selected from the solution that high molecular polymer forms; High molecular polymer comprises gum Arabic; Starch, carboxymethyl cellulose, methylcellulose, ethyl cellulose, polyethylene acetate fiber and polyethylene acetate fiber salt, Sodium Alginate, polyvinylidene chloride, polyethylene oxide, polyvinyl alcohol etc.; Preferably carboxymethyl cellulose solution, its concentration are 0.5%-3%.
4. the preparation method of false proof seed as claimed in claim 3; It is characterized in that; Described seed is plant seeds such as the vegetables that are fit to Pelleting, flowers, herbage, economic crops, vegetable seeds such as cauliflower, wild cabbage, rape etc., flower seed such as Malus spectabilis, petunia etc.; Grass seed such as alfalfa, lyme grass etc., economic crops such as tobacco, sesame etc.
5. the preparation method of false proof seed as claimed in claim 4; It is characterized in that; Said seed is preferably the seed that in actual production, needs through pill processing granule and minimum grain; Further preferred thousand kernel weight is less than the seed of 5g, and preferred especially thousand kernel weight is at the minimum grain seed of 0.05-0.5g.
6. like the preparation method of any described false proof seed of claim 1-5, it is characterized in that in granulation step, the gross mass that adds the first fluorescence toner is preferably the 0.45%-0.75% of naked mass; In the Pelleting step, the gross mass that adds the second fluorescence toner is preferably 5% or 10% or 15% of naked mass, and most preferably 10%.
7. the preparation method of false proof seed as claimed in claim 6 is characterized in that, plants the period of the day from 11 p.m. to 1 a.m when seed is a thousand kernel weight at the minimum grain of 0.05-0.5g, the 6-9 that the first kind of clothing agent quality that in granulation step, adds adds up to naked mass doubly, preferred 7.5 times; The second kind of clothing agent quality that in the Pelleting step, adds adds up to 35-43 times of naked mass, preferred 42 times; When granulation step finished, the particle diameter of minimum grain pelleted seed was 1.00mm-1.25mm, and when the Pelleting step finished, the particle diameter of minimum grain pelleted seed was 1.60mm-1.80mm.
8. detection method like the false proof seed of double fluorescent of claim 1 preparation, this method comprises the steps:
At first pelleted seed is placed on the slide; Add water and make its cracking; The pelleted seed that adds water-splitting with the blue light illumination of wave-length coverage 480nm～500nm; Show that as if pelleted seed under irradiation is inner bright green fluorescence then shines the pelleted seed of cracking then with the green glow of wave-length coverage 520nm～540nm; If the inner red fluorescence that becomes clear that shows of pelleted seed under irradiation, then described pelleted seed is the false proof seed of double fluorescent, does not have the branch of strict priority with blue light illumination with the step of green glow irradiation.
9. detection method like the false proof seed of double fluorescent of claim 1 preparation, this method comprises the steps:
Pelleted seed is sprouted; With the early stage seedling of the blue light illumination of wave-length coverage 480nm～500nm; If seedling can show bright yellow-green fluorescence under irradiation, then, under irradiation, show bright red fluorescence as if seedling then with the green glow irradiation of wave-length coverage 520nm～540nm; Then described pelleted seed is the false proof seed of double fluorescent, does not have the branch of strict priority with blue light illumination with the step of green glow irradiation.
10. detection method as claimed in claim 9; It is characterized in that, the tobacco pelleted seed is sprouted, with two cotyledons of the early stage seedling of the blue light illumination of wave-length coverage 480nm～500nm; If the most advanced and sophisticated and bright yellow-green fluorescence of stem growing point demonstration at cotyledon; Then then with the green glow irradiation of wave-length coverage 520nm～540nm, if the cotyledon vein shows bright red fluorescence under irradiation, then described pelleted seed is the false proof seed of double fluorescent.
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| CN108157369A (en) * | 2018-01-18 | 2018-06-15 | 浙江大学 | A kind of cold-resistant counterfeit-proof type seed coat agent and its application |
| CN108966748A (en) * | 2018-08-01 | 2018-12-11 | 玉溪中烟种子有限责任公司 | A kind of starch anti-counterfeiting tobacco coat pelleted seeds and preparation method thereof and identification method |
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