CN102608146A - Egg irradiation detection method - Google Patents
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- CN102608146A CN102608146A CN2011104114436A CN201110411443A CN102608146A CN 102608146 A CN102608146 A CN 102608146A CN 2011104114436 A CN2011104114436 A CN 2011104114436A CN 201110411443 A CN201110411443 A CN 201110411443A CN 102608146 A CN102608146 A CN 102608146A
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Abstract
The invention discloses an egg irradiation detection method, specifically comprising the following steps of: step a, taking out an egg shell as a sample; step b, dewatering the sample and crushing; step c, taking the sample with the preset weight in an ESR (Equivalent Series Resistor) instrument and collecting ESR wave spectrums; step d, judging ESR wave spectrum fracture factors and ESR wave spectrum graphics, and determining whether the egg is irradiated or not according to the ESR wave spectrum fracture factors and the ESR wave spectrum graphics. The egg irradiation detection method disclosed by the invention has the benefits that a pretreatment is simple without needing a chemical agent almost so as to prevent errors caused by residual chemical agent; an operation is simple, detection time is short, and result is obtained within 20-40s; and in addition, data reproducibility is strong as long as tuning is correct.
Description
Technical field
The present invention relates to a kind of irradiation detection method, especially a kind of egg irradiation detection method.
Background technology
Food irradiation processing is the key areas of Application of Nuclear Technology, and it utilizes ionising radiation rays such as gamma ray, X ray and electron beam and physical influence, chemical effect and the biological effect that the material effect produces to reach Pesticidal and sterilizing, prevents to go mouldy, suppresses plant germination, improves food hygiene quality, the purpose of maintenance nutritional quality and local flavor and prolongation shelf life.Because food irradiation processing has low energy consumption, pollution-free, noresidue and advantages such as safe and sanitary and cold working; Reducing the superiority that the aspect showed such as foodborne disease incidence, the loss in postpartum of reduction agricultural product, prolongation food shelf life; By the government department of more and more national and industrial sector cognition; At present existing a lot of state approvals hundreds of food can carry out irradiation treatment, food irradiation processing just progressively forms an emerging RADIATION PROCESSING industry.
Yet,, society is produced with sanitary condition the security through the food of irradiation processing worries because the feasible irradiated food detection method of food irradiation processing shortage system has had a strong impact on the testing of irradiated food.And, there is not the feasible irradiated food detection method of system to make to distinguish food through the various dose irradiation difficulty that becomes because different irradiation dose is also inequality to the effect that food produces.
Summary of the invention
To the problem of food irradiation processing shortage detection method, the present invention provides a kind of egg irradiation detection method.
The technological means that technical solution problem of the present invention is adopted is:
A kind of egg irradiation detection method wherein, specifically comprises the steps:
Step a, get egg eggshell as sample;
Step b, with grinding after the dehydration of said sample;
Step c, go the predetermined weight sample to place the ESR instrument, gather the ESR wave spectrum;
Steps d, the judgement ESR wave spectrum division factor and ESR wave spectrum figure confirm according to the wave spectrum division factor and ESR wave spectrum figure whether egg receives irradiation.
Above-mentioned egg irradiation detection method wherein, is got the method for egg eggshell and is beaten the egg method with beating eggs by hand for normal among the said step a, discard egg liquid and keep eggshell.
Above-mentioned egg irradiation detection method, wherein, the sample dehydration method is to place vacuum drying chamber with 30 ℃ temperature drying 12 hours among the said step b.
Above-mentioned egg irradiation detection method, wherein, the method that grinds sample among the said step b grinds for adopting the freeze grinding machine.
Above-mentioned egg irradiation detection method, wherein, the sample of predetermined weight is 0.5 g among the said step c.
Above-mentioned egg irradiation detection method, wherein, the ESR instrument among the said step c is an X-band, the internal diameter of ESR pipe is 5.0 mm.
Above-mentioned egg irradiation detection method, wherein, the running parameter of ESR instrument is among the said step c: magnetic field is set to central magnetic field 351.5 mT, field sweep width 20 mT; Microwave radiation is set to microwave frequency 9.5-10.0 GHz, power 4.9-5.1 mW; Signalling channel is set to time constant 40.96 ms, sweep times 20.48 s; Signal receives and is set to modulating frequency 100 kHz, modulated amplitude 0.5 mT, gain 10
3-10
4Temperature is set to room temperature.
Above-mentioned egg irradiation detection method, wherein, judge in the said steps d that the method for said ESR wave spectrum is: the egg without irradiation the ESR wave spectrum that signal intensity is lower and peak shape is mixed and disorderly relatively occurs after ESR detects; Typical asymmetry ESR wave spectrum appears in the egg through irradiation in magnetic field intensity 345-355 mT scope after ESR detects, mainly comprise two characteristic peaks: a characteristic peak and the characteristic peak that signal intensity is less that signal intensity is bigger.
Above-mentioned egg irradiation detection method, wherein, judge in the said steps d that the method for the said ESR wave spectrum division factor is:
Wave spectrum division factor g=
;
Wherein: ν
ESRBe microwave frequency, unit is GHz; B is a magnetic field intensity, the mT of unit;
, g judges that said sample is without irradiation when being 2.0054 ± 0.0002.
Above-mentioned egg irradiation detection method, wherein, the preparation control sample is used before detecting
60The Co gamma-rays shines egg respectively under room temperature, aerobic environment condition, producing irradiation dose is the control sample of 0.5,1,2,3,5 and 8 kGy, and will be without the sample of the irradiation control sample as 0 kGy; The control sample of 0,0.5,1,2,3,5 and 8 kGy is detected to the flow process among the step b with step a, the result that said detection is obtained as the sample detection of unknown irradiation dose with reference to foundation.
The invention has the beneficial effects as follows:
1. pre-treatment is simple, does not need chemical reagent basically, thereby can not bring the error that causes because of reagent is residual.
2. simple to operate, detection time is short, and 20-40 promptly goes out the result in second.
3. as long as tuning correct, data reappearance is strong.
Description of drawings
Fig. 1 is the process flow diagram of a kind of egg irradiation of the present invention detection method;
Fig. 2 is the ESR wave spectrum without the egg of irradiation;
Fig. 3 is that irradiation dose is the ESR wave spectrum of the egg of 1 kGy.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is described further, but not as qualification of the present invention.
As shown in Figure 1, a kind of egg irradiation of the present invention detection method wherein, specifically comprises the steps:
Step a, get egg eggshell as sample.Wherein, get the method for egg eggshell and can select to beat the egg method with beating eggs by hand normally, discard egg liquid and keep eggshell.Can adopt methyl alcohol-absolute ether (1:1) soaking and washing eggshell in case of necessity
Step b, with grinding after the dehydration of said sample.Wherein, the sample dehydration method can select to place vacuum drying chamber with 30 ℃ temperature drying 12 hours; The method that grinds sample can select to adopt the freeze grinding machine to grind.
Step c, go the predetermined weight sample to place the ESR instrument, gather the ESR wave spectrum.Wherein, the sample of predetermined weight is 0.5 g; The ESR instrument is an X-band, and the internal diameter of ESR pipe is 5.0 mm; The running parameter of ESR instrument is: magnetic field is set to central magnetic field 351.5 mT, field sweep width 20 mT; Microwave radiation is set to microwave frequency 9.5-10.0 GHz, power 4.9-5.1 mW; Signalling channel is set to time constant 40.96 ms, sweep times 20.48 s; Signal receives and is set to modulating frequency 100 kHz, modulated amplitude 0.5 mT, gain 10
3-10
4Temperature is set to room temperature.
Steps d, the judgement ESR wave spectrum division factor and ESR wave spectrum figure confirm according to the wave spectrum division factor and ESR wave spectrum figure whether egg receives irradiation.Wherein, wherein, judge that the method for ESR wave spectrum is: the egg without irradiation as shown in Figure 2 the ESR wave spectrum that signal intensity is lower and peak shape is mixed and disorderly relatively occurs after ESR detects; Typical asymmetry ESR wave spectrum appears in the egg through irradiation as shown in Figure 3 in magnetic field intensity 345-355 mT scope after ESR detects, mainly comprise two characteristic peaks: a characteristic peak and the characteristic peak that signal intensity is less that signal intensity is bigger.
Further, the method for the judgement ESR wave spectrum division factor is:
Wave spectrum division factor g=
;
Wherein: ν
ESRBe microwave frequency, unit is GHz; B is a magnetic field intensity, the mT of unit;
, g judges that said sample is without irradiation when being 2.0054 ± 0.0002.
Principle of the present invention is: the principal ingredient of egg shell is a lime carbonate, in accepting the irradiation process, makes CaCO in the eggshell
3When losing an electronics at the CO of crystallite kalzit
3 -Form lattice imperfection in the molecular structure, the electronics of release is by another CO
3 2-Catch and form an electronics center C O
3 3-CO
3 3-Radical life is longer, and the rate of decay is slower, contains unpaired electron, has the electron spin angular momentum, can be detected by ESR, forms distinctive ESR wave spectrum.Typical asymmetry ESR wave spectrum appears in the egg through irradiation as shown in Figure 3 in magnetic field intensity 345-355 mT scope after ESR detects, mainly comprise two characteristic peak: CO
3 3-Characteristic peak that the signal intensity of free-radical generating is bigger and CO
2 -The characteristic peak that the signal intensity of free-radical generating is less.Through 1kGy irradiation egg shell wave spectrum division factor g
1Value scope: g
1=2.0025 ± 0.0001, wave spectrum division factor g
2Value scope: g
2=1.9992 ± 0.0001.g
1Value is by CO
3 3-Free-radical generating, g
2Value is by CO
2 -Free-radical generating.ESR spectrogram peak height up and down is the ESR signal intensity, and characteristic peak highly then is up and down an ESR irradiation characteristic peak signal intensity.Adopt CO in the present invention
3 3-The characteristic peak that the signal intensity of free-radical generating is bigger carries out quantitative test.
Above-mentioned egg irradiation detection method, wherein, the preparation control sample is used before detecting
60The Co gamma-rays shines egg respectively under room temperature, aerobic environment condition; Producing irradiation dose is the control sample of 0.5,1,2,3,5 and 8 kGy; Can use the absorbed dose of each sample of silver dichromate quantimeter tracking and measuring, and will be without the sample of the irradiation control sample as 0 kGy; Control sample to 0,0.5,1,2,3,5 and 8 kGy detects with above-mentioned flow process, with the result who detect to obtain as the sample detection of unknown irradiation dose with reference to foundation.
The above is merely preferred embodiment of the present invention; Be not so limit claim of the present invention; So the equivalent structure that all utilizations instructions of the present invention and diagramatic content have been done changes, utilizes the material of mentioning same-actions such as tool among known and the present invention to replace; Utilize the means and methods of the same-actions of mentioning among known and the present invention such as means and methods tool to replace, resulting embodiment or result of implementation all are included in protection scope of the present invention.
Claims (10)
1. an egg irradiation detection method is characterized in that, specifically comprises the steps:
Step a, get egg eggshell as sample;
Step b, with grinding after the dehydration of said sample;
Step c, go the predetermined weight sample to place the ESR instrument, gather the ESR POP;
Steps d, the judgement ESR POP division factor and ESR wave spectrum figure confirm according to the wave spectrum division factor and ESR wave spectrum figure whether egg receives irradiation.
2. egg irradiation detection method according to claim 1 is characterized in that, the method for getting the egg eggshell among the said step a is beaten the egg method with beating eggs by hand for normal, discards egg liquid reservation eggshell.
3. egg irradiation detection method according to claim 1 is characterized in that, the sample dehydration method is to place vacuum drying chamber with 30 ℃ temperature drying 12 hours among the said step b.
4. egg irradiation detection method according to claim 1 is characterized in that, the method that grinds sample among the said step b grinds for adopting the freeze grinding machine.
5. egg irradiation detection method according to claim 1 is characterized in that the sample of predetermined weight is 0.5 g among the said step c.
6. egg irradiation detection method according to claim 1 is characterized in that the ESR instrument among the said step c is an X-band, and the internal diameter of ESR pipe is 5.0 mm.
7. egg irradiation detection method according to claim 1, it is characterized in that the running parameter of ESR instrument is among the said step c: magnetic field is set to central magnetic field 351.5 mT, field sweep width 20 mT; Microwave radiation is set to microwave frequency 9.5-10.0 GHz, power 4.9-5.1 mW; Signalling channel is set to time constant 40.96 ms, sweep times 20.48 s; Signal receives and is set to modulating frequency 100 kHz, modulated amplitude 0.5 mT, gain 10
3-10
4Temperature is set to room temperature.
8. like the said egg irradiation of claim 7 detection method, it is characterized in that judge in the said steps d that the method for said ESR wave spectrum is: the egg without irradiation the ESR wave spectrum that signal intensity is lower and peak shape is mixed and disorderly relatively occurs after ESR detects; Typical asymmetry ESR wave spectrum appears in the egg through irradiation in magnetic field intensity 345-355 mT scope after ESR detects, mainly comprise two characteristic peaks: a characteristic peak and the characteristic peak that signal intensity is less that signal intensity is bigger.
9. like the said egg irradiation of claim 7 detection method, it is characterized in that, judge in the said steps d that the method for the said ESR wave spectrum division factor is:
Wave spectrum division factor g=
;
Wherein: ν
ESRBe microwave frequency, unit is GHz; B is a magnetic field intensity, the mT of unit;
, g judges that said sample is without irradiation when being 2.0054 ± 0.0002.
10. like arbitrary said egg irradiation detection method among the claim 1-9, it is characterized in that the preparation control sample is used before detecting
60The Co gamma-rays shines egg respectively under room temperature, aerobic environment condition, producing irradiation dose is the control sample of 0.5,1,2,3,5 and 8 kGy, and will be without the sample of the irradiation control sample as 0 kGy; The control sample of 0,0.5,1,2,3,5 and 8 kGy is detected to the flow process among the step b with step a, the result that said detection is obtained as the sample detection of unknown irradiation dose with reference to foundation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891236A (en) * | 2014-12-15 | 2016-08-24 | 上海出入境检验检疫局动植物与食品检验检疫技术中心 | Fast technical method for identifying irradiation of anadara subcrenata and application thereof |
| CN105890966A (en) * | 2014-12-15 | 2016-08-24 | 上海出入境检验检疫局动植物与食品检验检疫技术中心 | Preparation technique and application for standard substance for identifying bone-containing irradiated food |
| CN106597515A (en) * | 2016-11-28 | 2017-04-26 | 江苏省农业科学院 | Product irradiation dose determination method |
| CN106772528A (en) * | 2016-11-28 | 2017-05-31 | 江苏省农业科学院 | A kind of irradiation of product dosage distribution and its assay method of unevenness |
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| CN1655869A (en) * | 2002-03-25 | 2005-08-17 | 住友钛株式会社 | Titanium oxide-based photocatalyst, manufacturing method therefor and its application |
| CN101241089A (en) * | 2008-03-11 | 2008-08-13 | 江苏省农业科学院 | Irradiation products discrimination method based on ESR method |
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Patent Citations (2)
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| CN1655869A (en) * | 2002-03-25 | 2005-08-17 | 住友钛株式会社 | Titanium oxide-based photocatalyst, manufacturing method therefor and its application |
| CN101241089A (en) * | 2008-03-11 | 2008-08-13 | 江苏省农业科学院 | Irradiation products discrimination method based on ESR method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891236A (en) * | 2014-12-15 | 2016-08-24 | 上海出入境检验检疫局动植物与食品检验检疫技术中心 | Fast technical method for identifying irradiation of anadara subcrenata and application thereof |
| CN105890966A (en) * | 2014-12-15 | 2016-08-24 | 上海出入境检验检疫局动植物与食品检验检疫技术中心 | Preparation technique and application for standard substance for identifying bone-containing irradiated food |
| CN106597515A (en) * | 2016-11-28 | 2017-04-26 | 江苏省农业科学院 | Product irradiation dose determination method |
| CN106772528A (en) * | 2016-11-28 | 2017-05-31 | 江苏省农业科学院 | A kind of irradiation of product dosage distribution and its assay method of unevenness |
| CN106597515B (en) * | 2016-11-28 | 2018-09-14 | 江苏省农业科学院 | A kind of assay method of irradiation of product dosage |
| CN106772528B (en) * | 2016-11-28 | 2020-04-14 | 江苏省农业科学院 | Method for measuring radiation dose distribution and nonuniformity of product |
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Application publication date: 20120725 |