CN102175745A - Method for quickly detecting fluorine content in specific vegetables - Google Patents
Method for quickly detecting fluorine content in specific vegetables Download PDFInfo
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Abstract
The invention discloses a method for quickly detecting fluorine content in specific vegetables. In the invention, an ion selective electrode method is used to detect the concentration content of fluoride in vegetables; Fluorine contents in leafy, root and tuber, and fruit vegetables from the majority of supermarket in Tianjin, and reasons of fluorine content difference in the vegetables are analyzed, wherein the fluorine content in common leafy vegetable is obviously higher than that in the other two vegetables, the main reason is probably that the leafy vegetable absorbs fluorine from the air and solid dust through pores on leaf surfaces during the growing process and the fluorine are enriched continually; meanwhile, fluorine content in green vegetables is far lower than that in the same common vegetables. The results show that the method for quickly detecting fluorine content in the specific vegetables is effective.
Description
Technical field
The invention belongs to the pesticide residue determination technical field, relate to the assay method of persticide residue in the agricultural product vegetables, fluorine fast Determination method in several vegetables of saying so more specifically.
Background technology
The food quality safety case is the important symbol of a national economic development level and people's living standard.Vegetables are as one of the most basic consumer goods, and its safety problem is related to whole its people's health.Therefore, the raw vegetable quality security problem has become the focus that the Chinese government and the common people pay close attention to, becomes the key factor that influences China's vegetables international competitiveness, continues to increase China's farmers' income.For a long time, heavy metal pollution is to influence one of principal element of agricultural products in China quality safety always.Use in a large number because of industry " three wastes " discharging and agricultural chemicals, chemical fertilizer in China vegetable plot, heavy metal pollution of soil is on the rise, this not only poisons soil-botanical system, reduce the victual quality, and by runoff and leaching polluted surface water and underground water, final direct, indirect hazard human life health.Heavy-metal residual is can't be with boiling or the method for soaking and washing is removed in vegetables, and its harm to human body is cumulative, latent period is long, and the people does not have symptom when just beginning, and is difficult at ordinary times discovering, will fall ill but be accumulated to a certain degree, and very serious once falling ill.
Fluorine is a trace element necessary in the human body, is to keep indispensable element in human growth, growth, the vital movement, and the average fluorinated volume of human body is about 37 μ g/g, and the human body fluorinated volume is too much or not enough, all can be unfavorable for health.It is 3.5mg that the fluorine for each person every day that China proposes allows intake, thus the intake that needs to control fluorine in certain scope to satisfy human body needs and unlikely generation deleterious effect.Vegetables are sources that a kind of main fluorine is taken in people's daily life, in most of city now, the supermarket becomes people's a more and more main food buying ground, and also have every day a large amount of vegetables to enter common family from the supermarket, so we should carry out strict control to quality and the contaminated degree of vegetables in the supermarket, and are healthy to guarantee broad masses of the people's.The content of fluoride of vegetables in the supermarket measured and analyze help us to understand the fluoride pollution degree of vegetables, very big realistic meaning is arranged.
Summary of the invention
The invention discloses fluorine fast Determination method in several vegetables, it is characterized in that being undertaken by following step:
(1) vegetables of gathering are dried to constant weight under 80 ℃, it is to be measured to put into exsiccator;
(2) extract:
1) 1.0mol/L sulfuric acid pipettes the 14ml concentrated sulphuric acid, uses distilled water diluting, uses the volumetric flask constant volume to 1L at last;
2) 0.2mol/L sodium citrate-1mol/L sodium nitrate: take by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up;
3) preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up standby;
(3) making of typical curve:
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml fluoride standard solution, place the 50ml volumetric flask, add the sulfuric acid extract that 10ml prepares, the 10ml damping fluid uses the distilled water constant volume to scale, standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stops to stir, read equilibrium potential E value, at last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope and related coefficient;
(4) mensuration of sample:
The vegetables of drying constant weight are smashed to pieces, taken by weighing 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate two minutes, add the 10ml damping fluid afterwards, measure the E value.
Method of the present invention, vegetables wherein are caraway, romaine lettuce, pakchoi, leek, lotus root, carrot, potato, eggplant, cucumber, green pepper, fresh kidney beans.
Method of the present invention, wherein the stirring rate in the step (3) is a 300-500 Zhuan ∕ branch.
Detailed assay method of the present invention is as follows:
1 development material
Vegetables such as the caraway of gathering in each main supermarket, Tianjin, romaine lettuce, pakchoi, leek, lotus root, carrot, potato, eggplant, cucumber, green pepper, fresh kidney beans are dried under 80 ℃ to constant weight (about two days), and it is to be measured to put into exsiccator.
2 development steps
2.1 extract
1.0mol/L sulfuric acid (H
2SO
4) pipette the 14ml concentrated sulphuric acid, use distilled water diluting, use the volumetric flask constant volume to 1L at last.
2.2 the total ionic strength adjustment buffer degree is regulated buffer solution (being abbreviated as TISAB):
0.2mol/L sodium citrate-1mol/L sodium nitrate takes by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up.
.2.3 fluoride standard solution
Preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up, and the content of fluorine ion just is 10 μ g/ml in the solution of this moment.
.2.4 the making of typical curve
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml the fluoride standard solution places the 50ml volumetric flask, adds the sulfuric acid extract that 10ml prepares, 10ml damping fluid (TISAB),, to scale standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration with the distilled water constant volume, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stop to stir, read equilibrium potential E value (noting: during mensuration, need by low concentration) to the high concentration sequentially determining.
At last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope (being the slope that influences of fluoride ion selective electrode) and related coefficient.
2.5 the mensuration of sample
The vegetables of drying constant weight are smashed to pieces, take by weighing about 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate two minutes, add 10ml damping fluid (TISAB) afterwards, measure the E value and (note: all want before each working sample to wash electrode approximately-350mv) with deionized water earlier to baseline potential
3 development results analyses
3.1 typical curve
Typical curve (1)
Regression line equation: E=58.79lgC – 270.95 coefficient R square be 0.9991
Typical curve (2)
Regression line equation: E=58.25lgC – 236.14 coefficient R square be 0.9999
3.2 the content of fluoride in the rhizome vegetable
Content of fluoride in table 3, the rhizome vegetable
Can clearly be seen that from the above-mentioned data that record the fluorine content in common potato, lotus root, the carrot these several big supermarkets will be higher than the fluorine content in the potato of nuisanceless class, lotus root, the carrot far away, it is lighter the fluoride pollution that vegetables that nuisanceless class has been described are subjected in the process of growth.Simultaneously fluorine content in the common lotus root and the fluorine content in the carrot all will be higher than fluorine content in the potato respectively in several big supermarkets, this mainly may have certain relation with the fluorine content in these three kinds of vegetables institute suitable growth soil, and also these three kinds of vegetables of possibility are relevant to the receptivity of fluorine in the environment.
3.3 the fluorine content of dish class vegetables
The fluorine content of table 4, dish class vegetables
The same with rhizome vegetable, fluorine content in each big supermarket in the common fruit vegetables all will be higher than non-harmful with the kind vegetables far away, and wherein the fluorine content in the eggplant is higher than fluorine content in other three kinds of vegetables again, and green pepper is that fluorine content is minimum in these four kinds of vegetables comparatively speaking.
3.4 the fluorine content of leafy vegetable
The fluorine content of table 5, leafy vegetable
Fluorine content in the leafy vegetable will be higher than the fluorine content in the preceding two class vegetables, and wherein the fluorine content in the common leafy vegetable is higher than fluorine content in the non-harmful vegetables of the same race again in each big supermarket, and caraway is the highest one of the fluorine content in these several vegetables.
4. development conclusion
The fluorine residue amount is not only relevant with soil fluorine content, but also may be relevant with fertilising situation, vegetables classification.We can find fluorine content in these tested vegetables than higher the data that draw more than seeing through, with regard to its reason, feel to mainly contain following some:
First: the chemical property of fluorine is more active, migration and accumulation in plant easily.
Second: the soil of planting vegetable often have soil fertility preferably, and the content of available nitrogen and available phosphorus also affects the contents level of fluorine in the vegetables in the soil.Its reason is that sufficient nutrient promotes that the vegetable growth metabolism is vigorous, photosynthesis and transpiration are all strengthened, and the water-soluble fluorine that vegetables absorb from soil transports to leaf portion with moisture by transpiration pull from root, metabolism in the accumulation of vegetable field top is also strengthened, so high fertilizer causes the high-load of fluorine.
The 3rd: the fluorine background value of some soil own is not high, but because ashes and the fertilizer of locals after burning is used with and applied the vegetable plot, makes in the vegetable plot water-soluble fluorine content than higher, thereby fluorine is run up in the plant product.These ectogenic fluorine often concentrate on soil surface, and are very high to the validity of plant, thereby make the fluorine in the vegetables be easy to accumulation.This phenomenon is more common in the rural area of China.This also is one of reason that influences vegetables fluorine content.
The 4th: a lot of relative concentrated areas, the vegetables place of production are distributed in around the cities and towns, the fluoride pollution that near during industry, rural area can be used the cities and towns coal burning produces, also affect upgrowth situation and the matter of some big Tanaka vegetables of periphery, this also is to cause the high factor of fluorine content in the vegetables.
We can find that clearly the content of fluoride in the vegetables of leaf class will be higher than content of fluoride in other two classes vegetables far away in to the comparison of tested a few class vegetables, in the same vegetables, fluorine at the general characteristic that various piece distributes is: the fluorine content in the leaf〉fluorine content in the fluorine content ≈ fruit in the piece root stem tuber.Reason may be after water-soluble fluorine is absorbed from root, arrives blade with the moisture transpiration pulling force, and moisture scatters and disappears from pore, and fluorine is finally stored in the vacuole of mesophyll cell after arriving leaf portion.In addition, the fluorine in the atmosphere also can advance blade and directly accumulates in leaf portion by pore.Wherein with regard to leaf vegetables different tissues organ, the distribution of fluorine is: the fluorine residue amount in the leaf〉fluorine residue amount in the root〉fluorine residue amount in the stem.
We are not difficult also to find that the fluorine content in the non-harmful vegetables all will be well below the fluorine content in the common vegetable of the same race simultaneously, the pollution level of this explanation pollution-free vegetable in the process of its growth has been subjected to relatively stricter control, wherein its fluoride pollution degree of being subjected to is lighter with respect to common similar vegetables, so we should select those nuisanceless when buying vegetables, the green vegetables that contaminated degree is lighter as far as possible.
At present, the problem that exceeds standard of less concern fluorine during the conventional vegetables of China detect.The background value of China's soil fluorine is (478+197.7) mg, and in south, the soil of planting vegetable is rice soil mostly, and the background value of its fluorine is often higher, is generally (5,33+,157 8) mg/kg.The high often fertile condition of growing vegetables is easy to cause exceeding standard of fluorine in the vegetables.Originally discover that the vegetables fluorine content of being taken a sample test generally exceeds standard, and has also illustrated this problem.Similarly situation is also commonplace on Xuzhou Area, Nanjing and other places.The nuisanceless production level of vegetables will improve in China, or enters the international market, must pay much attention to this problem.
Embodiment
For simple and purpose clearly, hereinafter appropriate omission the description of known technology, in order to avoid those unnecessary details influences are to the description of the technical program.The present invention is described further below in conjunction with example.
Embodiment 1
(1) with the pakchoi of gathering in the supermarket, under 80 ℃, dry to constant weight, it is to be measured to put into exsiccator;
(2) extract:
1) 1.0mol/L sulfuric acid pipettes the 14ml concentrated sulphuric acid, uses distilled water diluting, uses the volumetric flask constant volume to 1L at last;
2) 0.2mol/L sodium citrate-1mol/L sodium nitrate: take by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up;
3) preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up standby;
(3) making of typical curve:
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml fluoride standard solution, place the 50ml volumetric flask, add the sulfuric acid extract that 10ml prepares, the 10ml damping fluid uses the distilled water constant volume to scale, standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stops to stir, read equilibrium potential E value, at last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope and related coefficient;
(4) mensuration of sample:
The vegetables of drying constant weight are smashed to pieces, taken by weighing 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate two minutes, add the 10ml damping fluid afterwards, measure the E value.
Embodiment 2
(1) with the caraway of gathering in the supermarket, under 80 ℃, dry to constant weight, it is to be measured to put into exsiccator;
(2) extract:
1) 1.0mol/L sulfuric acid pipettes the 14ml concentrated sulphuric acid, uses distilled water diluting, uses the volumetric flask constant volume to 1L at last;
2) 0.2mol/L sodium citrate-1mol/L sodium nitrate: take by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up;
3) preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up standby;
(3) making of typical curve:
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml fluoride standard solution, place the 50ml volumetric flask, add the sulfuric acid extract that 10ml prepares, the 10ml damping fluid uses the distilled water constant volume to scale, standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stops to stir, read equilibrium potential E value, at last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope and related coefficient;
(4) mensuration of sample:
The vegetables of drying constant weight are smashed to pieces, taken by weighing 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate two minutes, add the 10ml damping fluid afterwards, measure the E value.
Embodiment 3
(1) with the carrot of gathering in the supermarket, under 80 ℃, dry to constant weight, it is to be measured to put into exsiccator;
(2) extract:
1) 1.0mol/L sulfuric acid pipettes the 14ml concentrated sulphuric acid, uses distilled water diluting, uses the volumetric flask constant volume to 1L at last;
2) 0.2mol/L sodium citrate-1mol/L sodium nitrate: take by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up;
3) preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up standby;
(3) making of typical curve:
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml fluoride standard solution, place the 50ml volumetric flask, add the sulfuric acid extract that 10ml prepares, the 10ml damping fluid uses the distilled water constant volume to scale, standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stops to stir, read equilibrium potential E value, at last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope and related coefficient;
(4) mensuration of sample:
The vegetables of drying constant weight are smashed to pieces, taken by weighing 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate two minutes, add the 10ml damping fluid afterwards, measure the E value.
Claims (3)
1. fluorine fast Determination method in several vegetables is characterized in that being undertaken by following step:
(1) vegetables of gathering are dried to constant weight under 80 ℃, it is to be measured to put into exsiccator;
(2) extract:
1) 1.0mol/L sulfuric acid pipettes the 14ml concentrated sulphuric acid, uses distilled water diluting, uses the volumetric flask constant volume to 1L at last;
2) 0.2mol/L sodium citrate-1mol/L sodium nitrate: take by weighing 58.8g Sodium Citrate, usp, Dihydrate Powder and 85g sodium nitrate, being dissolved in water changes in the volumetric flask of 1000ml, is diluted to graticule, shakes up;
3) preparation fluoride ion 100 μ g/ml sodium fluoride standard stock solutions pipette stock solution 10.00ml with the transfer pipet of 10ml more earlier, inject the 100ml volumetric flask, are diluted to graticule, shake up standby;
(3) making of typical curve:
Pipette 0.25 respectively with transfer pipet, 0.50,1.00,3.00,5.00,10.00ml fluoride standard solution, place the 50ml volumetric flask, add the sulfuric acid extract that 10ml prepares, the 10ml damping fluid uses the distilled water constant volume to scale, standard serial solution is transferred in the dried plastic beaker to high concentration successively by low concentration, electrode is inserted into detected solution, after starting stirrer 5-8 minute, stops to stir, read equilibrium potential E value, at last the data of gained are input in the computing machine intercept of the regression straight line of asking, slope and related coefficient;
(4) mensuration of sample:
The vegetables of drying constant weight are smashed to pieces, taken by weighing 1.0000g in the beaker of 50ml, add 10ml sulfuric acid extract, be put on the magnetic stirrer first lixiviate 2 minutes, add the 10ml damping fluid afterwards, measure the E value.
2. the described method of claim 1, vegetables wherein are caraway, romaine lettuce, pakchoi, leek, lotus root, carrot, potato, eggplant, cucumber, green pepper, fresh kidney beans.
3. the described method of claim 1, wherein the stirring rate in the step (3) is a 300-500 Zhuan ∕ branch.
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Cited By (6)
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| CN103424443A (en) * | 2013-05-28 | 2013-12-04 | 中国水稻研究所 | Ion-selective electrode method for measuring fluoride content in grains, vegetables and fruits |
| CN104713909A (en) * | 2015-04-10 | 2015-06-17 | 湖南农业大学 | Simple method for authenticating fluorine injury of plants |
| CN104884947A (en) * | 2012-12-21 | 2015-09-02 | 植物生物科学有限公司 | Soil chemistry sensor |
| CN105675698A (en) * | 2015-12-30 | 2016-06-15 | 辽宁工程技术大学 | Method of measuring bromine in coal with high temperature hydrolysis and bromine ion selective electrode |
| CN109813783A (en) * | 2019-03-28 | 2019-05-28 | 山东省产品质量检验研究院 | A kind of detection method improving wire and cable fluorine content measurement precision |
| CN114720534A (en) * | 2022-04-06 | 2022-07-08 | 山东省食品药品检验研究院 | Method for measuring fluorine in special medical food |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104884947A (en) * | 2012-12-21 | 2015-09-02 | 植物生物科学有限公司 | Soil chemistry sensor |
| CN104884947B (en) * | 2012-12-21 | 2018-01-09 | 植物生物科学有限公司 | Soil chemistry sensor |
| CN103424443A (en) * | 2013-05-28 | 2013-12-04 | 中国水稻研究所 | Ion-selective electrode method for measuring fluoride content in grains, vegetables and fruits |
| CN103424443B (en) * | 2013-05-28 | 2015-09-23 | 中国水稻研究所 | A kind of ion selecting electrode determining method of Oil repellent in grain, Vegetables and fruits |
| CN104713909A (en) * | 2015-04-10 | 2015-06-17 | 湖南农业大学 | Simple method for authenticating fluorine injury of plants |
| CN105675698A (en) * | 2015-12-30 | 2016-06-15 | 辽宁工程技术大学 | Method of measuring bromine in coal with high temperature hydrolysis and bromine ion selective electrode |
| CN109813783A (en) * | 2019-03-28 | 2019-05-28 | 山东省产品质量检验研究院 | A kind of detection method improving wire and cable fluorine content measurement precision |
| CN114720534A (en) * | 2022-04-06 | 2022-07-08 | 山东省食品药品检验研究院 | Method for measuring fluorine in special medical food |
| CN114720534B (en) * | 2022-04-06 | 2024-01-23 | 山东省食品药品检验研究院 | Method for determining fluorine in special medical food |
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Application publication date: 20110907 |