CN1309433C - Method for distinguishing agricultural products or food with radiation treatment or not - Google Patents
Method for distinguishing agricultural products or food with radiation treatment or not Download PDFInfo
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- CN1309433C CN1309433C CNB200510105986XA CN200510105986A CN1309433C CN 1309433 C CN1309433 C CN 1309433C CN B200510105986X A CNB200510105986X A CN B200510105986XA CN 200510105986 A CN200510105986 A CN 200510105986A CN 1309433 C CN1309433 C CN 1309433C
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Abstract
The present invention discloses a method for distinguishing agricultural products or foods with or without radiation treatment, which comprises the following steps: (1), carbonate in a sample to be measured is removed by hydrochloric acid, and organics in the sample to be measured are removed by H2O2 to obtain mineral substances of which the carbonate and the organics are removed; (2), the integral value of the peak area of a thermoluminescence light curve of the mineral substances of which the carbonate and the organics are removed is measured, and is represented by G1; then, after the mineral substances are irradiated by an irradiation dose of 1kGy, the integral value of the peak area of the thermoluminescence light curve of the mineral substances is measured again and is represented by G2. If the specific value of G1 and G2 is greater than or equal to 0.10, the sample to be measured is an agricultural product or food which is irradiated. If the specific value of the G1 and G2 is smaller than 0.10, the sample to be measured is the agricultural product or the food which is not irradiated. The method of the present invention has the advantages of high sensitivity, simple sample preparation, short detection period, no need of ground reference, high accuracy, etc.
Description
Technical field
The present invention relates to a kind of irradiation and method of irradiation agricultural product and food not distinguished, particularly a kind ofly distinguish the irradiation and the method for irradiation agricultural product and food not with the thermoluminescence analytical method.
Background technology
Food irradiation is a kind of novel foodstuff preservation technology that emerges after the World War II, apart from the history of modern existing over half a century.It is that ionising radiation is used for food storage to physics, chemistry and the biological effect of material effect, reaches desinsection, sterilization, sprout inhibition, delays maturation, quarantine control parasitic infection and improve the purpose of hygienic quality.Because that food irradiation has is energy-conservation, efficient is high, do not heat up, safe and reliable and keep advantage such as the good organoleptic quality of food, be again to the traditional food process technology replenish and perfect, in current food processing and preservation field, show extremely wide prospect.Along with international trade globalization and the business-like fast development of irradiated food, more and more countries and tissue increase (Grolichova M day by day to the degree of concern whether food passes through irradiation, Dvorak P, MusilovaH.Employing Ionizing Radiation to Enhance Food Safety-a Review.Acta Vet.Brno, 2004,73:143-149; Lutter R.Food Irradiation--The Neglected Solutionto Food-Borne Illness.Science, 1999,286:2275-2281; Chen Qixun. Chinese food irradiation progress, Beijing: the Atomic Energy Press, 1998:1-21).Therefore, the research of irradiated food detection method is also imperative.This is not only the needs of consumer's right to know, still eliminates the international trade technology barriers and promotes the business-like needs of irradiated food.
Under International Atomic Energy Agency supports and organizes, the irradiated food detection technique has been carried out than extensive studies.The method that can be used for detecting irradiated food at present mainly contains: electron spin resonance, high performance liquid chromatography, gas-matter on-line method, the thermoluminescence luminescence method, laser imaging detection method, nine kinds of method (J Raffi such as dna cleavage product detection method, M Kent.Method of identification of irradiated foodstuffs, in:L.Nollet (Ed.) .Handbook of Food Analysis, Marcel Dekker.New York, 1996:1889-1906).These methods mostly are to cause physics, chemistry, biology and physiology variation in the food to be carried out according to irradiation.Especially the mineral matter in Sanderson discovery at end of the eighties in last century food is actually thermoluminescent source, all to contain mineral remaining because all are exposed to food in soil or the dust storm, theoretically, nearly all agricultural product all available heat are released the optical analysis detection, the superiority and the broad applicability of this method more highlight, and this technology also has object of reference, the single-minded and highly sensitive characteristics of irradiation of need not.But along with the raising of living standards of the people and enterprise's working ability, the mineral pollution source of seasoner products is fewer and feweri, and existing extraction process is difficult to satisfy the needs that thermoluminescence is analyzed.
Utilize the thermoluminescence analytic approach to distinguish irradiation and not irradiated food and agricultural product, at first just need the extraction mineral matter.Impurity such as organic matter that is mingled with in the mineral matter that extracts and carbonate can make the thermoluminescence curve " burr " peak occur, cause integrated value bigger than normal; Add that the responsiveness of carbonate crystal in two scopes of low dosage and high dose is different, also can bring than mistake to result of the test.Therefore, remove that organic matter and carbonate are the committed steps of extracting mineral matter in the experiment material, result of the test is had bigger influence.
Summary of the invention
The purpose of this invention is to provide a kind of irradiation and method of irradiation agricultural product and food not distinguished.
The differentiation irradiation provided by the present invention and the method for irradiation agricultural product and food not may further comprise the steps:
1) removes carbonate in the testing sample with hydrochloric acid, use H
2O
2Remove the organic matter in the testing sample, carbonate and organic mineral matter are removed;
2) measure described peak area integrated value of removing the thermoluminescence luminosity curve of carbonate and organic mineral matter, with G
1The expression, then with this mineral matter behind the irradiation dose irradiation of 1kGy, measure the peak area integrated value of its thermoluminescence luminosity curve again, with G
2Expression; As G
1With G
2Ratio more than or equal to 0.10, then this testing sample is by irradiated agricultural product or food, as G
1With G
2Ratio less than 0.10, then this testing sample is not for by irradiated agricultural product or food.
The testing sample of agricultural product can be taken from the surperficial rinse thing of agricultural product, any position that also can take from agricultural product.
The desirable any part of the testing sample of food from food.
The granular size of removing carbonate and organic mineral matter can directly influence the inhomogeneities of dosage absorption, and too small particle has very strong skin effect, makes the thermoluminescence overflow, and excessive particle surface effect is too small, make the thermoluminescence signal excessively a little less than.In order to obtain the suitable thermoluminescence signal of intensity, in the described method, also be included in and obtain removing in the step 1) after carbonate and the organic mineral matter, with described step 2) before, to the step that carbonate and organic mineral matter carry out following flotation of removing that obtains in the step 1): remove carbonate and organic mineral matter with what obtain in the deionized water suspension step 1), after leaving standstill 5-10 minute, remove precipitation, after upper strata liquid left standstill 1-2 hour, remove upper strata liquid, the precipitation that obtains be particle diameter be 3-8 μ m remove carbonate and organic mineral matter.
Described hydrochloric acid is general chemistry reagent, and weight percent concentration is 36%.
Described H
2O
2Be general chemistry reagent, weight percent concentration is 30%.
The peak area integrated value of described thermoluminescence luminosity curve is the peak area integrated value in 150 ℃ of-260 ℃ of intervals.
The measurement parameter of described thermoluminescence luminosity curve is: SA=4.56, D=2, F=2; 15 ℃ of programming rate per seconds; The 1st time of staying 8s, temperature remains on 135 ℃; The 2nd time of staying 12s, temperature remains on 350 ℃.
The present invention combines the direct rinse of water surface method with direct acidifying with oxidation, remove carbonate and organic matter in the testing sample, the organic matter and the carbonate that influence the peak area integrated value have been removed, the error of result of the test is reduced greatly, and do not adopt expensive sodium tungstate solution to handle, reduced cost; The present invention by flotation obtain particle diameter be 3-8 μ m evenly pure remove carbonate and organic mineral matter, make the intensity of thermoluminescence signal suitable, make that test repeatability is strong, the result is accurate.Method of the present invention has highly sensitive, and sample preparation is simple, and sense cycle is short, and need not use object of reference, high accuracy for examination.Method of the present invention can be used for detecting the food that can isolate mineral matter and whether pass through radiation treatment, and is particularly particularly suitable to agricultural product.
Description of drawings
Fig. 1 is the G of 85 samples
1/ G
2Statistical chart.
Fig. 2 is without the peppery thermoluminescence first luminosity curve G in the irradiation
1
Fig. 3 is without the peppery thermoluminescence second luminosity curve G in the irradiation
2
Fig. 4 is the thermoluminescence first luminosity curve G through the irradiation potato
1
Fig. 5 is the thermoluminescence second luminosity curve G through the irradiation potato
2
The specific embodiment
The described method of following examples is conventional method if no special instructions.
Embodiment 1, distinguish the irradiated food and the method for irradiated food not
One, separation and Extraction mineral matter
RGD-3 thermoluminescence analyzer (Anti-Chemical Defence Research Inst. PLA); KQ-100 supersonic generator (Kunshan Ultrasonic Instruments Co., Ltd.); LD4-2 low speed centrifuge (Beijing Medical Centrifugal Machine Factory); SG-202 electrically heated drying cabinet (Shen, Shanghai light instrument and meter Co., Ltd).It is pure that the experiment agents useful for same is analysis.
Potato (free market purchase) is divided into two parts, and wherein a part (1) is without irradiation, and another part (2) is through 0.1kGy irradiation; In peppery (U.S. total eclipse product Co., Ltd) without irradiation; Soup on the seafood (hundred fragrant Food Co., Ltd) is through 10kGy irradiation; Barley seedling powder (Hengshui wheat seedling powder factory) is through 6kGy irradiation; Pollen (honeybee research institute of the Chinese Academy of Agricultural Sciences) is through 4kGy irradiation.
1, the mineral matter that has a large amount of mineral soil agricultural product-potato sample separates and extracts: water rinse potato sample surfaces, washing lotion is collected in the beaker, leave standstill 24 hours after, slowly inclining supernatant, connects beaker and precipitation is put into 50-60 ℃ of drying in oven together.Then, dried deposit sample is put into mortar grind (preventing that local temperature is too high) gently, cross 200 mesh sieves, the sample under the sieve is poured beaker into.Because the mineral samplers complicated component, wherein organic matter and carbonate are bigger to the thermoluminescence effect of signals, must remove with the method for acidifying and oxidation.With sample acidifying and oxidation under the above-mentioned mistake 200 mesh sieves sieve, process is as follows: add the hydrochloric acid (excessive) of 10ml deionized water and 10ml 36% in the beaker that fills the 10g soil sample, add 20ml 30% H behind the stirring 10min
2O
2(excessive) leaves standstill reaction 24 hours, adds deionized water then to brimmer, and inclining every 4 hours supernatant liquor and add deionized water again, and 4-5 time so repeatedly, to supernatant pH=7.Because test adopts the particulate method to survey thermoluminescence, the size of particulate can directly influence the inhomogeneities that dosage absorbs, and too small particulate has very strong skin effect, makes the thermoluminescence overflow.According to Stokes' law, the flotation fine particle diameter is 3-8um.So carry out flotation, floatation process is: the soil sample acidified and oxidation removal organic matter and carbonate, add deionized water to brimmer, and shake up, leave standstill 10min, at the bottom of being deposited to glass greater than the particle of 8um,, left standstill again 1 hour another beaker of upper strata liquid impouring.Inclining then upper strata liquid, and the sediment of beaker bottom promptly is that diameter is the particulate of 3-8um.Use acetone (analyzing pure) to transfer in the small beaker at last, staticly settle, discard acetone solution, the mineral matter that precipitates is put into 50-60 ℃ of drying in oven together with small beaker, take by weighing 5mg and put into sample cell, treat measurement of thermoluminescence.
2, the mineral matter of spice, dehydrated vegetables sample separates and extracts: get among the 100g peppery respectively, soup on the seafood, barley seedling powder, pollen sample, directly acidifying and oxidation as follows: add the hydrochloric acid (excessive) of 50ml 36%, add 100ml 30%H behind the stirring 10min
2O
2(excessive), and handle with the 30KHz ultrasonic wave staticly settled 4 hours afterwards, discard behind the organic matter of upper strata centrifugal, abandoning supernatant, collecting precipitation thing.Sediment is carried out flotation with the method for step 1 flotation.Obtain 5mg mineral matter sample, treat the thermoluminescence analysis to measure.
Two, the thermoluminescence luminosity curve is measured
The sample mineral matter extract that step 1 obtains is evenly poured into respectively in the thermoluminescent measurement shallow bid, opened RGD-3 thermoluminescence analyzer.The apparatus measures parameter is chosen for: SA=4.56, D=2, F=2; 15 ℃ of programming rate per seconds; The 1st time of staying 8s, temperature remains on 135 ℃; The 2nd time of staying 12s, temperature remains on 350 ℃.Glow peak is got the peak area integrated value in 150 ℃ of-260 ℃ of intervals.The luminosity curve that measures is first luminosity curve, uses G
1Expression peak area integrated value.Again this was measured G
1Sample all collect and carry out irradiation in the sample cell, irradiation devices adopt Atomic Energy Utilization Inst. of China Agricultural Sciences Academy
60Co γ irradiation bomb, dosage are 1kGy, and dosimeter adopts the silver dichromate dosimeter.Carry out the measurement of thermoluminescence second time then under similarity condition again, the luminosity curve that obtains is second luminosity curve, uses G
2Represent this peak area integrated value.It is as shown in table 1 that the thermoluminescence of sample is analyzed data:
The thermoluminescence analytical data of the different testing samples of table 1
| Sample | One-shot measurement | Secondary is measured | G 1/G 2 | The irradiation situation |
| G 1 | G 2 | |||
| Potato (1) | 354500 | 7185700 | 0.049 | Irradiation not |
| Potato (2) | 1146100 | 5696300 | 0.200 | According to mistake |
| In peppery | 419000 | 10048400 | 0.040 | Irradiation not |
| Soup on the seafood | 1329100 | 1041100 | 1.280 | According to mistake |
| Barley seedling powder | 583800 | 720800 | 0.800 | According to mistake |
| Pollen | 1376400 | 2769500 | 0.500 | According to mistake |
The result shows: irradiation sample is compared the peak area integrated value ratio (G of luminosity curve with irradiation sample not
1/ G
2) data difference be significantly, the G of two of irradiation samples not wherein
1/ G
2All be far smaller than 0.10, and the G of 4 samples of irradiation
1/ G
2All greater than 0.10.With reference to the employing actual dose of food irradiation both at home and abroad, the precision that detects according to measuring instrument itself is set every irradiation dose (comprises 0.10kGy) more than 0.10kGy food simultaneously, regards as irradiated food; If food itself or wherein have certain auxiliary material to accept irradiation dose less than 0.10kGy assert that then food do not accept irradiation.So, after the mineral matter that extracts in the sample is accepted irradiation dose 1kGy, the ratio G of the peak area integrated value of its luminosity curve
1/ G
2If less than 0.10, judge that then food do not accept irradiation, and ratio is more little, the possibility of acceptable dose is just more little; G
1/ G
2If more than or equal to 0.10, judge that then sample is irradiated, and ratio is big more, acceptable dose is just high more.
Without first and second luminosity curve of thermoluminescence such as Fig. 2 and Fig. 3 of peppery in the irradiation.Long-pending 419000 (the G that are respectively of the peak area of first and second luminosity curve between 150 ℃ to 260 ℃
1) and 10048400 (G
2), G
1/ G
2=0.040; And the curve shape of the two has apparent in view difference, can judge that this sample do not accept irradiation, conforms to actual conditions.Through first and second luminosity curve of thermoluminescence of potato (2) sample of irradiation as shown in Figure 4 and Figure 5.According to the test operation condition, the long-pending 1146100 (G that are respectively of the peak area of first and second luminosity curve between 150 ℃ to 260 ℃
1) and 5696300 (G
2), G
1/ G
2=0.20; And the curve shape of the two is more similar, can judge that potato is irradiated sample, conforms to actual conditions.From two picture groups, more as can be known, on first luminosity curve of sample, all have many " burrs ", and basic the maintenance smoothly on second luminosity curve.The pure degree of the mineral matter that extracts in the appearance of burr and the sample has very confidential relation, and the impurity that the mineral matter of extraction contains (mainly being organic matter and carbonate) is many more, and the possibility that burr occurs is just big more.Can be so that the most of ashing of impurity under the high temperature of degree more than 200 at the phase I mineral matter, irradiation doses then, second luminosity curve that obtains is just essentially smooth; But a low temperature peak can occur along with temperature raises gradually under less than 150 ℃ condition, this is to capture the result that more shallow electronics is at first overflowed behind the sample irradiation doses.
Therefore, for accuracy and the validity that proves this detection criteria, in 6 big based foods to the permission irradiation of national regulation, chosen solid-state and food liquid, and do, 85 samples such as fresh fruit vegetables extract mineral matter with the described method of step 1 respectively, have carried out the thermoluminescence check and analysis, wherein 45 samples are accepted the irradiation dose that actual process needs, the result shows 45 irradiation samples after the thermoluminescence analyzer detects, G as shown in Figure 1
1/ G
2Ratio all greater than 0.1, differentiate accuracy and reach 100%; 40 not irradiation sample after identifying, 38 not irradiation sample G are arranged
1/ G
2Ratio all less than 0.1,2 not G of irradiation sample are arranged
1/ G
2Ratio be equal to 0.1, differentiate accuracy and reach 95%.Statistics draws a qualitative judgement foundation at last: promptly, work as G
1/ G
2〉=0.10 o'clock, judge that sample is irradiated, and ratio is big more, it is just big more to accept irradiation dose; And G
1/ G
2＜0.10 o'clock, judge that sample is an irradiation not, ratio is more little, and the possibility of accepting irradiation is just more little.
Claims (6)
1, a kind of irradiation and method of irradiation agricultural product and food not distinguished may further comprise the steps:
1) removes carbonate in the testing sample with hydrochloric acid, use H
2O
2Remove the organic matter in the testing sample, what make particle diameter and be 3-8 μ m removes carbonate and organic mineral matter;
2) measure described peak area integrated value of removing the thermoluminescence luminosity curve of carbonate and organic mineral matter, with G
1The expression, then with this mineral matter behind the irradiation dose irradiation of 1kGy, measure the peak area integrated value of its thermoluminescence luminosity curve again, with G
2Expression; As G
1With G
2Ratio more than or equal to 0.10, then this testing sample is by irradiated agricultural product or food, as G
1With G
2Ratio less than 0.10, then this testing sample is not for by irradiated agricultural product or food.
2, method according to claim 1, it is characterized in that: the described particle diameter that makes is the step that the method for removing carbonate and organic mineral matter of 3-8 μ m comprises following flotation: remove carbonate and organic mineral matter with what obtain in the deionized water suspension step 1), after leaving standstill 5-10 minute, remove precipitation, after upper strata liquid left standstill 1-2 hour, remove upper strata liquid, the precipitation that obtains be particle diameter be 3-8 μ m remove carbonate and organic mineral matter.
3, method according to claim 1 and 2 is characterized in that: the weight percent concentration of described hydrochloric acid is 36%.
4, method according to claim 1 and 2 is characterized in that: described H
2O
2Weight percent concentration be 30%.
5, method according to claim 1 and 2 is characterized in that: the peak area integrated value of described thermoluminescence luminosity curve is the peak area integrated value in 150 ℃ of-260 ℃ of intervals.
6, method according to claim 1 and 2 is characterized in that: the measurement parameter of described thermoluminescence luminosity curve is elected as: SA=4.56, D=2, F=2; 15 ℃ of programming rate per seconds; The 1st time of staying 8s, temperature remains on 135 ℃; The 2nd time of staying 12s, temperature remains on 350 ℃.
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| CN100407939C (en) * | 2006-07-02 | 2008-08-06 | 宁波超能科技股份有限公司 | Additive method for reducing fish food or fish powder radiation sterilizing dosage |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5606163A (en) * | 1995-01-11 | 1997-02-25 | The United States Of America As Represented By The Secretary Of The Navy | All-optical, rapid readout, fiber-coupled thermoluminescent dosimeter system |
| JPH11302641A (en) * | 1998-04-17 | 1999-11-02 | Read:Kk | Monoclinic hydroxide phosphor and its production |
| CN1292709A (en) * | 1998-02-05 | 2001-04-25 | 梅迪斯卡恩有限公司 | Method for irradiating item with electron radiation |
| CN1584556A (en) * | 2004-06-16 | 2005-02-23 | 中科古物鉴证实验室有限公司 | Method for determining age of porcelain after Song Dynasty by light emitting after heating |
-
2005
- 2005-10-08 CN CNB200510105986XA patent/CN1309433C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5606163A (en) * | 1995-01-11 | 1997-02-25 | The United States Of America As Represented By The Secretary Of The Navy | All-optical, rapid readout, fiber-coupled thermoluminescent dosimeter system |
| CN1292709A (en) * | 1998-02-05 | 2001-04-25 | 梅迪斯卡恩有限公司 | Method for irradiating item with electron radiation |
| JPH11302641A (en) * | 1998-04-17 | 1999-11-02 | Read:Kk | Monoclinic hydroxide phosphor and its production |
| CN1584556A (en) * | 2004-06-16 | 2005-02-23 | 中科古物鉴证实验室有限公司 | Method for determining age of porcelain after Song Dynasty by light emitting after heating |
Non-Patent Citations (2)
| Title |
|---|
| 辐照食品分析检测技术的研究进展 哈益明 周洪杰，食品科学，第26卷第6期 2005 * |
| 食品辐照与辐照食品的检测 秦志荣 等，食品工业，第2期 2000 * |
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