CN107247049B - A kind of test paper for detecting cadmium content in cereal with screening agent - Google Patents
A kind of test paper for detecting cadmium content in cereal with screening agent Download PDFInfo
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- CN107247049B CN107247049B CN201710436969.7A CN201710436969A CN107247049B CN 107247049 B CN107247049 B CN 107247049B CN 201710436969 A CN201710436969 A CN 201710436969A CN 107247049 B CN107247049 B CN 107247049B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The test paper of cadmium content in the detection cereal that the present invention relates to a kind of with screening agent, the test paper from top to bottom successively include solid layer, color layer, support base and solid layer, and support base is additionally equipped with standard color comparison card；The support base is the filter paper with screening agent and sensitizer；The solid layer is two layers, and two layers of solid layer is to have the xanthan gum with screening agent and sensitizer；The color layer is the compound color developing agent of cadmium.The present invention has test paper with middling speed quantitative filter paper for basic backing material, cheap and easy to get, easy to carry.The advantages that main support object filter paper outer layer of test paper is covered to form diaphragm by xanthan gum, plays the role of protection and fixed color developing agent, increases the shelf-life of test paper.
Description
Technical field
The invention belongs to detect cadmium ion content technical field in cereal, and in particular to the invention belongs to detect cadmium in cereal
Ion concentration technical field, and in particular to the method and test paper of cadmium ion in a kind of quick detection cereal with screening agent.
Background technique
In recent years, with industry, agricultural, the fast development of the industries such as processing industry, the pollution problem of heavy metal has been in environment
Increasingly aggravate.And the heavy metal in environment can constantly be accumulated by food chain, jeopardize the existence and health of the mankind, such as Hunan
Cadmium rice event.And cadmium content excessive aggregation can make muscular atrophy in human body, textured bone, have an effect on enzyme system in liver kidney organ
Normal function, when serious can because hepatorenal syndrome death.And the probability that women can be made to suffer from breast cancer of taking in for a long time of cadmium increases
Add.It therefore, is the content of heavy metal cadmium in control grain, it is necessary to which, to the water quality in grain producing region, soil and process carry out
Monitoring, and establish quickly, the convenient method suitable for on-site test cadmium ion is particularly important.
Currently, commonly the analysis method of detection heavy metal cadmium ion has a ultraviolet spectrophotometry, atomic absorption spectrography (AAS),
Atomic emission spectrometry, electrochemical process, inductively coupled plasma mass spectrometry.Ultraviolet spectrophotometry is multiple due to test process
It is miscellaneous, stability and less reproducible, and other methods high sensitivity when analyzing cadmium ion content, error are small, as a result accurately, but
Large-scale instrument and professional operator are needed, the detection period is long, and it is complicated for operation, and expensive equipment, it is not suitable for live fast
Speed detection.
It retrieves and finds by existing technical literature, the Chinese patent that number of patent application is 201410021261.1 is entitled
The test paper of detection Chinese herbal medicine cadmium content with screening agent, the test paper which is invented includes the tape test successively overlapped
Hole, the sample-adding substrate of control wells, the fibrous layer of the glass with screening agent and have two at reaction substrate with cadmium color developing agent
For a peephole respectively with instrument connection, control wells are corresponding.It is colour developing using p-nitrophenyl diazonium azobenzene and its homologous series substance
Agent, by color developing agent, Substrate Protection agent, excipient, sensitizer is dried in vacuo after buffer grinding, on being coated on reaction substrate.
Sample liquid is added dropwise in instrument connection, phosphate buffer is added dropwise in control wells, practical colour developing degree and colorimetric card is compareed, to examine
Measure out rapid determination of content of cadmium element in Chinese herbal medicine.Screening agent is fixed on test paper by the test paper for the first time, easy to carry, but the disadvantage is that system
It is cumbersome to make process, test paper is made of four layers of backing material, and extemporaneous preparation phosphate buffer solution is needed to do pair during the test
According to.
The research in relation to detecting cadmium ion test paper domestic at present is less, and Triazene used in the present invention is being done
Biggish technological difficulties are how color developing agent is fixed on the support carrier when at test paper, and such organicvisualization reagent generally exists
Dissolubility in water is poor.Less with the remaining color developing agent of the test paper of its alcohol solution dipping institute, detection limit does not meet detection
It is required that larger using limitation.
Summary of the invention
It is an object of the invention to improve in view of the drawbacks of the prior art, a kind of detection with screening agent is provided
The test paper of cadmium content in cereal.It is solid agent that the test paper, which is firstly introduced xanthan gum, and has adsorption effect, and production is simple, operation
Convenient, specificity is good, and high sensitivity, detection time is short, low in cost, and property is stablized, and limited period reaches half a year, does not need large-scale expensive
Weight instrument auxiliary, suitable for field quick detection, and detection process does not need to reduce environmental pollution using phosphoric acid.
To achieve the goals above, according to the test paper of cadmium content in detection cereal provided by the invention, including following technology
Scheme:
A kind of test paper for detecting cadmium content in cereal with screening agent, the test paper from top to bottom successively include solid
Layer, color layer, support base and solid layer, support base are additionally equipped with standard color comparison card；The support base is with masking
The filter paper of agent and sensitizer；The solid layer is two layers, and two layers of solid layer is to have the xanthan gum with screening agent and sensitizer；Institute
Stating color layer is the compound color developing agent of cadmium.
Further, the screening agent of the support base and solid layer is mixed masking agent, including hydroxylamine hydrochloride, amino second
Acid, stone acid sodium and thiocarbamide；The sensitizer be triton x-100, emulsifier op-10 or Tween-20 any one.
Further, the support base and solid layer use the additive amount of screening agent: each component is respectively 0.5-1 grams.
Further, the compound color developing agent of the cadmium is that mesoporous silicon sphere loads 2- hydroxyl -5- sulfonic group phenyldiazonium amino azo
Benzene cadmium, the compound color developing agent of cadmium in 100 milligrams of mesoporous silicon spheres the preparation method comprises the following steps: be added 3 milliliters of 2- hydroxyl -5- sulfonic group
Phenyldiazonium aminoazabenzol ethanol solution, the concentration of 2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol are 1 milligram/milli
It rises, adds 7mL deionized water, be protected from light and 32h is stirred at room temperature, the shape in 20 milliliters of deionized water is redissolved in centrifugation after the completion of loading
At compound chromogenic reagent solution.
Further, the preparation of the support base includes the following steps: that the screening agent each component is taken to be dissolved in respectively
Masking agent solution is formed in ionized water, sensitizer is added, filter paper is impregnated in above-mentioned solution 20 minutes, is taken out, vacuum drying.
Further, the preparation of the color layer includes the following steps: base's filter paper will be supported to be laid in Buchner funnel, takes 1
The compound chromogenic reagent solution of milliliter makes compound color developing agent stay in branch support group on the support base filter paper of fixed size range after suction filtration
On layer filter paper.
Further, the preparation of the solid layer include the following steps: to take respectively the screening agent each component be dissolved in from
Masking agent solution is formed in sub- water, is added sensitizer, is taken 20 milliliters of solution of screening agent and sensitizer, 20 milligrams of Huangs are added
The colloid is evenly coated in the support base for being fixed with compound color developing agent by virgin rubber, heating stirring to colloid uniform bubble-free respectively
The upper surface of filter paper and the lower surface of support base's filter paper, form solid layer.
Further, the filter paper is middling speed quantitative analysis filter paper, low speed quantitative analysis filter paper or ordinary filter paper.It selects such
Backing material, the material of cellulose makes compound color developing agent be easier to stay in support base, and such material is cheap and easy to get, very
Big degree reduces costs.
Further, the standard color comparison card is the cadmium-ion solution for preparing series of standards concentration, its pH is transferred to
11.30 or so, under the conditions of this pH, the color developing agent of compound color developing agent and cadmium ion is most obvious, and test paper is separately immersed in this
15 minutes in the cadmium-ion solution of series, color is taken, standard color range is fabricated to.
The invention also discloses the test paper of cadmium content in this detection cereal with screening agent detection cereal in cadmium contain
The application of amount.
Hydroxylamine hydrochloride in the formula of screening agent, amion acetic acid be mainly used for shelter copper ion, cobalt ions, nickel ion, iron from
The interference of son and zinc ion；Sodium potassium tartrate tetrahydrate, thiocarbamide are mainly used for sheltering silver ion, mercury ion, copper ion, lead ion etc. it is dry
It disturbs.
The present invention is stayed compound color developing agent on the support base filter paper of fixed area using filtering for the first time, then compound
Xanthan gum is smeared on color developing agent, successfully compound color developing agent is fixed on filter paper, and by screening agent and sensitizer with more
Easy method introduces test paper, test paper cadmium content suitable for field quick detection cereal.It establishes in on-site test cereal
The new method of cadmium ion.Compared with prior art, this method has the advantage that
1, test paper with middling speed quantitative filter paper be basic backing material, it is cheap and easy to get, it is easy to carry.
2, the main support object filter paper outer layer of test paper is covered to form diaphragm by xanthan gum, plays protection and fixes color developing agent
Effect, increases the shelf-life of test paper.
3, test paper manufacturing process is simple, is combined using filtering with xanthan gum, by compound color developing agent fixation a on filter paper,
It is suitable for producing in enormous quantities, and production cost is low.
4, easy to operate, most of reagent required for measuring is fixed on test paper, and detection process does not need to add again
Enter, and does not need to reduce environmental pollution using phosphoric acid.
5, detection sensitivity high specific is strong.When test paper of the invention being recycled quickly to detect the cadmium content in grain, inspection
Rising limit is 0.1ppm, and accuracy in detection is not much different with atomic absorption spectrophotometry substantially.Due to the introduction of screening agent, for
The masking of other metal ions has good effect, to improve the specificity of detection.
6, it is widely used.Test paper established by the present invention can be applied to: grain, soil, water quality, processed food,
The detection of cadmium content in the substances such as Chinese herbal medicine, cosmetics.Furthermore above-mentioned sample has to pass through digestion process before testing, by chemical combination
The cadmium element of state is digested to inorganic cadmium ion, then is measured.
Detailed description of the invention:
Fig. 1 is the device figure of cadmium content test paper in the quick detection cereal with screening agent.
Wherein, 1- solid layer, 2- support base, 3- color layer.
Specific embodiment
In order to make the purpose of the present invention, technical solution and advantage are more clearly understood, below in conjunction with attached drawing and example, to this
Invention is further elaborated.And specific example described herein is used only for explaining the present invention, is not used to limit
The present invention.Without departing from the inventive concept of the premise, the similar improvement that can be done, belongs in the scope of the present invention.
Embodiment 1
Test paper structure of the invention is simple, only using filter paper as basic backing material, and will successfully be shown using xanthan gum
The composite material of toner is fixed on filter paper, is below exactly the manufacturing process of the test paper:
1 cadmium color developing agent and mesoporous silicon sphere it is compound: selected silicon ball is the mesoporous silicon sphere of diameter 50nm or so, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol ethanol solution, 2- hydroxyl -5- sulphur are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized water, is protected from light and 32h is stirred at room temperature, and is filled
Centrifugation is redissolved after the completion of carrying forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
The mixed solution of 2 preparation screening agents, sensitizer: hydroxylamine hydrochloride, amion acetic acid, wine are added in 90mL deionized water
Stone acid potassium sodium, each 1g of thiocarbamide after being completely dissolved, add Qula and lead to 110-X10mL, ultrasound is completely dissolved to Qula is logical, spare.
3 preparations contain screening agent, the mixed colloidal solution of xanthan gum: sensitizer takes the matched screening agent of 20mL2, sensitizer
Mixed solution, be added 20mg xanthan gum, heating stirring to colloid uniform bubble-free.
The preparation of 4 test paper: uniformly by the compound chromogenic reagent solution ultrasound of cadmium obtained in 1, take 1mL in fixed size range
Filtered on filter paper, stay in composite material on filter paper, take matched mixed colloidal solution in 0.5mL3 later, be uniformly coated in containing
On the filter paper of color developing agent composite material, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, it again will after vacuum drying
There is no the filter paper part of color developing agent to cut, is sealed, the test paper of cadmium content in the detection cereal as invented.
The preparation of 5 standard color ranges:
The ammonium hydroxide of 3mL10% is added in 25mL volumetric flask, the pH of solution is 11.30 or so at this time, is configured to a series of
Then the cadmium standard solution of concentration is clapped the color of test paper with digital camera by the test paper made bubble 15 minutes in standard liquid
Under, go out colorimetric card using Photoshop7.0 software design on computers, and mark out corresponding detectable concentration range, prepares
At standard color range.The detection range of this test paper is 0.1~10ppm.
Embodiment 2
1 cadmium color developing agent and mesoporous silicon sphere it is compound: selected silicon ball is the mesoporous silicon sphere of diameter 50nm or so, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol ethanol solution, 2- hydroxyl -5- sulphur are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized water, is protected from light and 32h is stirred at room temperature, and is filled
Centrifugation is redissolved after the completion of carrying forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
2 prepare screening agent, the mixed solution of sensitizer: hydroxylamine hydrochloride 0.5g, amino second being added in 90mL deionized water
Acid 0.5, sodium potassium tartrate tetrahydrate 0.5, each 1g of thiocarbamide after being completely dissolved, add emulsifier op-10 10mL, ultrasound to emulsifier
OP-10 is completely dissolved, spare.
3 preparations contain screening agent, the mixed colloidal solution of xanthan gum: sensitizer takes matched screening agent, enhanced sensitivity in 20mL2
20mg xanthan gum, heating stirring to colloid uniform bubble-free is added in the mixed solution of agent.
The preparation of 4 test paper: uniformly by the compound chromogenic reagent solution ultrasound of cadmium obtained in 1, take 1mL in fixed size range
Filtered on filter paper, stay in composite material on filter paper, take matched mixed colloidal solution in 0.5mL3 later, be uniformly coated in containing
On the filter paper of color developing agent composite material, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, it again will after vacuum drying
There is no the filter paper part of color developing agent to cut, is sealed, the test paper of cadmium content in the detection cereal as invented.
The preparation of 5 standard color ranges:
The ammonium hydroxide of 3mL10% is added in 25mL volumetric flask, the pH of solution is 11.30 or so at this time, is configured to a series of
Then the cadmium standard solution of concentration is clapped the color of test paper with digital camera by the test paper made bubble 15 minutes in standard liquid
Under, go out colorimetric card using Photoshop7.0 software design on computers, and mark out corresponding detectable concentration range, prepares
At standard color range.The detection range of this test paper is 0.1~10ppm.
Embodiment 3
1 cadmium color developing agent and mesoporous silicon sphere it is compound: selected silicon ball is the mesoporous silicon sphere of diameter 50nm or so, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol ethanol solution, 2- hydroxyl -5- sulphur are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized water, is protected from light and 32h is stirred at room temperature, and is filled
Centrifugation is redissolved after the completion of carrying forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
2 prepare screening agent, the mixed solution of sensitizer: hydroxylamine hydrochloride 1g, amion acetic acid being added in 90mL deionized water
0.6, sodium potassium tartrate tetrahydrate 1, each 0.5g of thiocarbamide after being completely dissolved, adds Tween-20 10mL, and ultrasound is completely molten to Tween-20
Solution, it is spare.
3 preparations contain screening agent, the mixed colloidal solution of xanthan gum: sensitizer takes matched screening agent, enhanced sensitivity in 20mL2
20mg xanthan gum, heating stirring to colloid uniform bubble-free is added in the mixed solution of agent.
The preparation of 4 test paper: uniformly by the compound chromogenic reagent solution ultrasound of cadmium obtained in 1, take 1mL in fixed size range
Filtered on filter paper, stay in composite material on filter paper, take matched mixed colloidal solution in 0.5mL3 later, be uniformly coated in containing
On the filter paper of color developing agent composite material, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, it again will after vacuum drying
There is no the filter paper part of color developing agent to cut, is sealed, the test paper of cadmium content in the detection cereal as invented.
The preparation of 5 standard color ranges:
The ammonium hydroxide of 3mL10% is added in 25mL volumetric flask, the pH of solution is 11.30 or so at this time, is configured to a series of
Then the cadmium standard solution of concentration is clapped the color of test paper with digital camera by the test paper made bubble 15 minutes in standard liquid
Under, go out colorimetric card using Photoshop7.0 software design on computers, and mark out corresponding detectable concentration range, prepares
At standard color range.The detection range of this test paper is 0.1~10ppm.
The measurement of cadmium content in embodiment 4, rice meal
The digestion pre-treatment of sample: using mixed acid wet digestion, takes 3 kinds of rice meals by being ground up, sieved, and crosses 80 mesh
Sieve, weighs 2g sample and is placed in beaker in tall form, and 10mL concentrated nitric acid, soaked overnight is added, and 160 DEG C of heating, which disappear to boil to solution, becomes clear,
Increase chloric acid 5mL and continue to disappear and boil to clear, continues to be heated to acid solution amount about 2mL, the lead standard liquid 1mL of 2.1ppm is added, with ammonium hydroxide tune
Saving pH value of solution is about 11.30, is settled to 25mL in the ammonium hydroxide-ammonium chloride buffer solution for being about 11.30 with pH.
The detection of actual sample: the Test paper invented being immersed in the digestion solution of three of the above rice, and 15 minutes
The color of test paper and standard color comparison card compare afterwards, and testing result indicates, are not detected in three portions of rice.For above-mentioned molten
Liquid uses inductance coupled plasma-Mass Spectrometer Method, testing result 0.094ppm, 0.0207ppm, 0.2736ppb again.Two kinds
Testing result is consistent substantially, illustrates that invented Test paper meets the requirements.
The measurement of cadmium content in embodiment 5, mung bean flour
In this example, 3 kinds of different mung bean flours is selected to carry out digestion process.To the processing method of sample with embodiment 4
It is identical.
The detection basic step of sample is identical with example 4.Testing result shows that the testing result of 3 parts of mung bean flours is two parts
It being not detected, a content is 0.1ppm, with inductance coupled plasma-Mass Spectrometer Method, testing result 0.1365ppb,
0.1454ppb, 0.1312ppm.
It is that specific example of the present invention is described above.In addition, the invention is not limited to above-mentioned specific implementations
Mode, the deformation or modification made within the scope of the claims to the present invention, does not affect the essence of the present invention.This hair
Bright Test paper production process is simple, low in cost, easy to use, can be widely used in on-site test, before development
Scape is wide.
Claims (9)
1. the test paper of cadmium content in a kind of detection cereal with screening agent, which is characterized in that the test paper is from top to bottom successively
Including solid layer, color layer, support base and solid layer, support base is additionally equipped with standard color comparison card；The support base is
Filter paper with screening agent and sensitizer；The solid layer is two layers, and two layers of solid layer is with screening agent and sensitizer
Xanthan gum；The color layer is the compound color developing agent of cadmium, and the compound color developing agent of cadmium is that mesoporous silicon sphere loads 2- hydroxyl -5- sulfonic group
Phenyldiazonium aminoazabenzol cadmium, the compound color developing agent of cadmium in 100 milligrams of mesoporous silicon spheres the preparation method comprises the following steps: be added 3 milliliters
2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol ethanol solution, 2- hydroxyl -5- sulfonic group phenyldiazonium aminoazabenzol
Concentration be 1 mg/ml, add 7mL deionized water, be protected from light and 32h is stirred at room temperature, load after the completion of centrifugation redissolve in 20 milli
The compound chromogenic reagent solution of cadmium is formed in the deionized water risen.
2. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, which is characterized in that institute
The screening agent for stating support base and solid layer is mixed masking agent, including hydroxylamine hydrochloride, amion acetic acid, stone acid sodium and thiocarbamide；
The sensitizer be triton x-100, emulsifier op-10 or Tween-20 any one.
3. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 2, which is characterized in that institute
State support base and solid layer uses the additive amount of screening agent: each component is respectively 0.5-1 grams.
4. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 3, which is characterized in that institute
The preparation for stating support base includes the following steps: that taking the screening agent each component to be dissolved in deionized water respectively forms screening agent
Solution adds sensitizer, and filter paper is impregnated in above-mentioned solution 20 minutes, takes out, vacuum drying.
5. the test paper of cadmium content, feature exist in a kind of detection cereal with screening agent according to claim 1 or 3
In the preparation of the color layer includes the following steps: base's filter paper will be supported to be laid in Buchner funnel, takes 1 milliliter of compound colour developing
Agent solution on the support base filter paper of fixed size range, make after suction filtration compound color developing agent stay in support base's filter paper on.
6. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 3, which is characterized in that institute
The preparation for stating solid layer includes the following steps: to take the screening agent each component to be dissolved in deionized water respectively, and to form screening agent molten
Liquid adds sensitizer, takes 20 milliliters of solution of screening agent and sensitizer, 20 milligrams of xanthan gum, heating stirring to glue is added
The colloid is evenly coated in the upper surface for being fixed with support base's filter paper of compound color developing agent and support by body uniform bubble-free respectively
The lower surface of base's filter paper forms solid layer.
7. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, which is characterized in that institute
Stating filter paper is middling speed quantitative analysis filter paper, low speed quantitative analysis filter paper or ordinary filter paper.
8. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, which is characterized in that institute
The standard color comparison card stated is the cadmium-ion solution for preparing series of standards concentration, its pH is transferred to 11.30, test paper is soaked respectively
Bubble takes color, is fabricated to standard color range 15 minutes in this series of cadmium-ion solution.
9. a kind of a kind of test paper for detecting cadmium content in cereal with screening agent according to any one of claims 1 to 8
The application of cadmium content in detection cereal.
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| CN109668875A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院大连化学物理研究所 | It is a kind of for quickly detecting the test paper of pesticide sevin |
| CN112683889B (en) * | 2020-12-04 | 2023-01-17 | 西安建筑科技大学 | Binary chromogenic test paper and method for rapidly and semi-quantitatively detecting Cd (II) |
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