CN108507862A - A kind of Cadmium detrmination method in animal's liver - Google Patents
A kind of Cadmium detrmination method in animal's liver Download PDFInfo
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- CN108507862A CN108507862A CN201810283804.5A CN201810283804A CN108507862A CN 108507862 A CN108507862 A CN 108507862A CN 201810283804 A CN201810283804 A CN 201810283804A CN 108507862 A CN108507862 A CN 108507862A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The present invention relates to a kind of Cadmium detrmination methods in animal's liver, the assay method includes the preparation of animal's liver sample to be tested, cadmium Specification Curve of Increasing, sample pre-treatments, Specimen Determination and quantitative calculating, it is improved by the digestion procedure to traditional sample pre-treatments, animal's liver sample to be measured is cleared up using transparent and with a scale polyolefin digestion tube, the constant volume directly in the digestion tube, operating procedure is not only simplified, and reduces operating procedure and the operating error in washing transfer constant volume process and pollution.Animal's liver sample to be tested solution after pernitric acid and hydrogen peroxide steeped overnight is just transparent, and it need to be 60 DEG C~90 DEG C in temperature to be placed in after electric heating resolution instrument only, and heating digestion time is 1h~2h just enough.Verified, using the method to its calibration curve coefficient correlation value higher of the measurement of animal's liver sample, method detection limit 0.012mg/kg, precision is more preferable, and recovery of standard addition meets the requirements, can be with large-scale promotion application.
Description
Technical field
The invention belongs to heavy-metal residual detection technique fields, more particularly, to Cadmium detrmination side in a kind of animal's liver
Method.
Background technology
China is the consumption big country of pluck.With the continuous improvement of living standards of the people, people are to edible animal
The safety and sanitation situation pay attention to day by day of food.While livestock and poultry breeding industry and culture fishery in China obtain continuing to develop,
Because the harmful components that the links of cultivation enter in animal body cause serious threat to the health of the mankind, and heavy metal is residual
Stay even more can by feeding environment, feed processing, butcher the various approach of processing and act on animal body, and then it is strong to endanger the mankind
Health.Along with feeding environment pollution increasingly sharpens, the reasons such as growth accelerator are excessively used in producer, the heavy metals such as cadmium can be dynamic
It is enriched in object histoorgan.As the vitals of metabolism, liver carries the important process of organism detoxication and toxicant eliminating function, right
Cadmium in animal's liver is measured, and measured value can reflect animal by heavy metal pollution degree.
The quantitative detecting method of heavy metal has：It is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), atomic fluorescence
Method (AFS), inductively coupled plasma method (ICP), X fluorescence spectrum (XRF), Inductively coupled plasma-mass spectrometry (ICP-MS).
Currently, the measurement of cadmium in foods generally uses GB 5095.15-2014《The measurement side of national food safety standard cadmium in foods
Method》The content of various cadmium in foods is measured, pressure dispelling can be used in the resolution processing before sample measures in the method
Tank resolution method, micro-wave digestion, Wet digestion or dry ashing method, corresponding digestion container are that polytetrafluoroethylene (PTFE) clears up inner canister, micro-
Wave counteracting tank, conical flask or porcelain crucible.
Conventional pressure counteracting tank resolution method, Wet digestion and dry ashing method resolution method have some universal defects：
(1) digestion time is long；
(2) digestion condition is higher；
(3) complex for operation step, repeatedly washing transfer constant volume, is also easy to produce operating error and pollution, influences measurement result.
Micro-wave digestion has the advantages that resolution is complete, quick, low latitude is white, but since the interpolation of microwave current counteracting tank is cleared up
Tank is typically also that translucent or opaque material is also required for rinsing counteracting tank, then shifts solution after resolution
To volumetric flask constant volume, thus the resolution method there is also complex for operation step, multiple washing transfer constant volume, be also easy to produce operating error and
Pollution and the defect for influencing measurement result.Therefore, simplicity carried out to the content of beary metal of animal's liver, quickly and accurately measured,
It has important practical significance to animal food market safety Health Administration and safe edible.
Invention content
For this reason, it may be necessary to a kind of Cadmium detrmination method in animal's liver be provided, to solve traditional cadmium continuous mode resolution processing
Time is long, digestion condition is high and because counteracting tank/pipe is not visible and can not directly constant volume due to need to repeatedly wash transfer constant volume and produced
Raw measurement result error problem.
To achieve the above object, a kind of Cadmium detrmination method in animal's liver, the assay method packet are inventor provided
It includes：
Animal's liver sample to be tested prepares and cadmium Specification Curve of Increasing；
Sample to be tested pre-treatment, Specimen Determination and quantitative calculating；
The sample to be tested pre-treatment step includes：
Weigh the animal's liver sample to be tested being ready for, be placed in can be read volume data and can constant volume transparent resolution hold
In device, strong acid and strong oxidizer is added, stands, then is placed in heat resolution instrument to heat by the digestion container and clear up, resolution knot
Continue to be heated to tobacco ease to the greatest extent after beam, takes out the digestion container, add matrix modifier after cooling, being diluted to this with purified water disappears
Container constant volume graduation mark is solved, shakes up, animal's liver sample is made, it is to be measured；
The Specimen Determination is the cadmium absorbance for measuring the animal's liver sample, described to be quantitatively calculated as animal's liver
The cadmium absorbance value of Specimen Determination corresponds to cadmium standard curve progress cadmium concentration and quantitatively calculates.
During tradition measures, the digestion procedure selected according to laboratory condition has：(1) pressure dispelling tank resolution method；(2) microwave
Resolution method；(3) Wet digestion；(4) dry ashing method.Using any one digestion procedure in these four, it is required for clearing up, catching up with
After acid terminates, digestion solution is moved into volumetric flask, then washs digestion container for several times with salpeter solution, washing lotion is merged into capacity
Bottle, mixing constant volume is spare, during multiple washing, merging and mixing, is easy, because operating instrument and step are various, to cause to try
Sample has generated error before entering sampling Graphite Furnace Atomic Absorption spectrophotometer, influences final measuring result.Therefore, digestion container
Transparent visual and can direct constant volume, resolution terminate it is cooling after directly into digestion container addition matrix modifier and with pure
Change water and be diluted to the scale for needing constant volume, has important practical significance for accurate measure of the simplicity of heavy-metal residual.
In sampling Graphite Furnace Atomic Absorption analysis, in order to increase the volatility of testing sample solution matrix, or improve to be measured easy
The stability of volatile element, and certain chemical reagent is added in testing sample solution, it is eliminated with allowing raising ashing temperature
Or reducing Matrix effects, this chemical reagent is referred to as matrix modifier.
Further, the digestion container is polyolefins digestion tube, and the polyolefin includes polyethylene, polypropylene, gathers
It is one or more in 1- butylene and poly(4-methyl-1-pentene).
Polyolefin is by alpha-olefins such as ethylene, propylene, 1- butylene, 1- amylenes, 1- hexenes, 1- octenes, 4-methyl-1-pentenes
And certain cycloolefins be polymerized alone or combined polymerization obtained from a kind of thermoplastic resin general name.It can be by adding the systems such as auxiliary agent
For odorless, nontoxic, feel ceraceous, with excellent high and low temperature resistance, chemical stability, high fondant-strength, high transparency, Gao Jie
The polymer of brilliant degree and impact strength, for manufacture film, container, pipeline, chemical apparatuses, electronic device, insulating materials and
Medical apparatus.Using including one kind or more in polyethylene, polypropylene, poly 1-butene and poly(4-methyl-1-pentene) in the present invention
Kind be that digestion tube made from material clears up animal's liver sample, breach significantly traditional polytetrafluoroethylene (PTFE) resolution inner canister,
The bottleneck of micro-wave diminishing pot, conical flask or porcelain crucible in resolution makes digestion process become accurate, easy and time saving.
Further, the constant volume of the digestion container ranging from 1mL~100mL.
The volume specification of digestion container is selected according to animal's liver sample to be tested sampling amount, and experimental determination is generally selected
The digestion tube of 10mL, 25mL and 50mL.
Further, the heat resolution instrument is that electric heating clears up instrument or bath clears up instrument.
Since the digestion process of the present invention is relatively low relative to the temperature heated needed for traditional digestion procedure, it can adopt
Instrument is cleared up with electric heating or bath clears up instrument.
Further, the animal's liver sample to be tested is dry-eye disease or fresh sample, if animal's liver sample to be tested is dry
The dry-eye disease is then ground into the uniform powder that grain diameter is less than 40 mesh by sample, is stored in clean container, and carry out mark
Note, saves backup；If animal's liver sample to be tested is fresh sample, which is broken into homogenate, is stored in clean container
In, and mark, it is saved backup in freezing equipment.
Further, 300~600g of animal's liver powder to be measured or homogenate is weighed, using quartering division to 60g
~120g, it is spare.
Sample quarterlies are called conical quartering, refer to that every sample piles uniform cone, and is pressed into frustum, then use
Cross frame is divided into a kind of division operating method of the quartering.The method is early in 50 generation of 19th century by Sweden scholar VonPost
The quadrat method founded, and extensive use.Sample is required according to measurement levigate, crosses the sieve of certain pore size, then mix, put down
It is paved into circle, is divided into the quartering, takes opposite two parts to mix, then divides equally again, until reaching the requirement of oneself.Concrete operations rise
It to depend on the circumstances, if sample is liquid, mixing, first mixing be facilitated to sample again；Sample is solid, finely ground, and mixing is equal
Even sampling.The percent similarity of sample quarterlies, no matter with relative aboundance, relative frequency, relative dominance or importance value
As quantitative data, it is all higher than 65%.After the animal's liver powder to be measured of the present invention or homogenate are mixing, using quartering
It is sampled, then the animal's liver sample to be tested taken can represent the overall condition of the animal's liver.
Further, the strong acid be nitric acid, addition be 3.0mL~6.0mL, the strong oxidizer be hydrogen peroxide or
Perchloric acid, addition are 1.0mL~3.0mL.
Nitric acid is most common acid with strong oxidizing property in resolution, and in addition to Au, Pt, almost other metal salts can be dissolved in nitre
Acid, it is good to the discomposing effect of protein, xanthoproteic test occurs, generates the nitroprotein easily aoxidized.Perchloric acid can almost divide
All organic matters are solved, and decomposition rate is fast, but be not used alone generally, is often used together with nitric acid.The energy of oxidation of hydrogen peroxide
Power with solution acidity enhance and enhance, usually with a concentration of 30% hydrogen peroxide.Single oxidizing acid is not easy in operation
Sample is decomposed completely or easy tos produce danger, is used in combination frequently with two or more oxidants or oxidizing acid day, it is each to play
Self-applying is cleared up with enabling organic matter high-speed smooth.Preferred nitric acid-the hydrogen peroxide of the present invention or nitric acid-perchloric acid system are to dynamic
Object liver specimens are cleared up, the sample containing alcohol, glycerine or lipid organic matter should first with nitric acid dousing longer time, keep its complete
At a degree of resolution, pellucidity is presented in liquid.
Further, the heating resolution is carried out in the following conditions：Temperature is 60 DEG C~90 DEG C, heats digestion time
For 1h~2h, continue to be heated to nitrogen dioxide tobacco ease to the greatest extent after resolution.
Since the object that the present invention is measured is animal's liver sample, through pernitric acid-hydrogen peroxide or the high chlorine of nitric acid-
After acid system impregnates, substantially resolution finishes for alcohol, glycerine or lipid organic matter in sample, therefore, as long as 60 DEG C~
Heating resolution 1h~2h can clear up completely at a temperature of 90 DEG C.
Further, the described matrix modifier of addition is ammonium dihydrogen phosphate, and additive amount is 0.5mL~2mL.
Common matrix modifier has ammonium dihydrogen phosphate, palladium nitrate, magnesium nitrate.In the present invention, it is due to measuring target
Cadmium, boiling point is relatively low, and ammonium dihydrogen phosphate is added as matrix modifier to reduce Matrix effects, makes measurement result closer to reality
Content.
Further, which is characterized in that the absorbance value measurement is carried out in the following conditions：Wavelength 228.8nm,
Lamp current 2mA~10mA, 105 DEG C, drying time 20s~30s of drying temperature, 400 DEG C~700 DEG C of ashing temperature, ashing time
20s~40s, 1300 DEG C~2300 DEG C of atomization temperature, atomization time 3s~5s.
Absorbance measurement is according to GB in the absorbance value measurement and the manufacturing process of cadmium standard working curve
The method of 5095.15-2014 carries out.
In addition, in order to verify accuracy, the precision of technical solution of the present invention, method is given in preferential embodiment
Detection limit, precision values and recovery of standard addition are worth results of measuring.
It is different from the prior art, above-mentioned technical proposal has the following advantages that：
(1) animal's liver sample to be measured is cleared up using transparent and with a scale polyolefins digestion tube, is cleared up
After without being washed to digestion tube, cleaning solution be transferred to volumetric flask again carry out constant volume, but directly in the digestion tube
Interior constant volume not only simplifies operating procedure, and reduces the operating error in operating procedure and washing transfer constant volume process；
(2) in sample pre-treatments of the invention, animal's liver sample to be tested solution after pernitric acid and hydrogen peroxide dipping
Just transparent, it need to be 60 DEG C~90 DEG C in temperature to be placed in after heat resolution instrument only, and heating digestion time is 1h~2h just enough enough,
With traditional in thermostatic drying chamber, 12 DEG C~160 DEG C digestion 4h~6h of temperature are compared, and are reduced digestion temperature, are shortened and disappear
Change the time, the risk of operating personnel's acid mist sucking is substantially reduced, conducive to safely and fast cadmium is provided to animal's liver sample to be measured
Examining report.
Description of the drawings
Fig. 1 is the cadmium standard curve made by present embodiment.
Specific implementation mode
For the technology contents of technical solution, construction feature, the objects and the effects are described in detail, below in conjunction with specific reality
Example is applied to be explained in detail.
Embodiment one
The present embodiment provides a kind of Cadmium detrmination method in animal's liver, which includes the following steps：
Animal's liver sample to be tested prepares：Fresh Liver of Ctenopharyngodon Idellus 600g is weighed, homogenate is broken into beater, is used
Above-mentioned Liver of Ctenopharyngodon Idellus is homogenized division to 120g by quartering, is contained in clean beaker, and mark, -16 in refrigerator
It DEG C saves backup；
Instrument reagent prepares：The electric heating that temperature controlling range is 0 DEG C~300 DEG C clears up instrument, weighing accuracy to 0.0001g
Assay balance, beater, the atomic absorption spectrophotometer with nickel light source, graphite furnace, ashless filter paper, 50mL polythene PEs disappear
Solution pipe and temperature can be transferred to -16 DEG C of refrigerator；
1% nitric acid, 1+1 hydrochloric acid, 30% hydrogen peroxide, 10g/L ammonium dihydrogen phosphates, 1000mg/L cadmiums standard reserving solution,
100ng/mL cadmiums standard solution, acetylene and cadmium content be respectively 0ng/mL, 0.50 ng/mL, 1.0ng/mL, 1.5ng/mL,
The cadmium standard curve working solution of 2.0ng/mL, 3.0ng/mL.
All reagents and instrument and equipment occurred in the present embodiment can prepare or acquisition purchased in market.
Sample pre-treatments：The Liver of Ctenopharyngodon Idellus homogenate that 5.0g is ready for is weighed, is placed in 50mL polythene PE digestion tubes,
3.0mL nitric acid and 1.0mL hydrogen peroxide is added, stands overnight, the polythene PE digestion tube, which is then placed in electric heating, clears up instrument
In, in 80 DEG C of heating resolution 1.5h, temperature is improved after resolution and continues to be heated to nitrogen dioxide tobacco ease to the greatest extent to 110 DEG C, is taken
Go out the polyethylene digestion tube, adds 1mL ammonium dihydrogen phosphates after cooling, determining for the polyethylene digestion tube is diluted to deionized water
Scale is measured, shakes up, Liver of Ctenopharyngodon Idellus sample is made, it is to be measured；
Cadmium Specification Curve of Increasing：Absorbance value measurement is carried out in the following conditions：Wavelength 228.8nm, lamp current 5mA,
105 DEG C of drying temperature, drying time 30s.700 DEG C of ashing temperature, ashing time 40s；2300 DEG C of atomization temperature, when atomization
Between 3s.It respectively takes 20uL to inject graphite furnace by the sequence of concentration from low to high standard curve working solution, then draws 5uL and survey its extinction
Angle value, with a concentration of abscissa of standard curve working solution, corresponding absorbance value is ordinate, with the various concentration of 5 points
Cadmium standard solution draw standard curve and find out the unary linear regression equation of absorbance value and concentration relationship.
Specimen Determination：Under the identical experiment condition of bioassay standard curve working solution, pipette samples digestive juice 20uL, note
Enter graphite furnace, surveys its absorbance value.The content that cadmium in treatments of the sample liquid is sought in the unary linear regression equation of standard series is substituted into,
Parallel determination number is no less than twice.If measurement result exceeds standard curve range, carried out after being diluted with salpeter solution (1%)
It measures.
Cadmium content is calculated by formula (1) in the Liver of Ctenopharyngodon Idellus sample：
In formula：
The content of nickel in X- samples, unit are ng/kg (μ g/kg)；
A1- measures the content of nickel in sample liquid, and unit is nanograms per milliliter (ng/mL)；
The content of nickel in A2- blank solutions, unit are nanograms per milliliter (ng/mL)；
V- sample constant volumes, unit are milliliter (mL)；
The quality of m- samples, unit are gram (g)；
1000- conversion coefficients.
Embodiment two
The present embodiment provides a kind of Cadmium detrmination method in animal's liver and embodiment one the difference is that：
Animal's liver sample to be tested prepares：Australia dragon design spot liver dry-eye disease 300g is weighed, is broken into grinder
Even powder, and 40 mesh sieve is crossed, using quartering by above-mentioned Australia dragon design spot liver powder division to 60g, it is contained in clean, dry
Medicine bottle in, and mark preservation, it is spare；
Instrument reagent prepares：The bath that temperature controlling range is 0 DEG C~200 DEG C clears up instrument, weighing accuracy to 0.0001g
Assay balance, grinder, the atomic absorption spectrophotometer with nickel light source, graphite furnace, ashless filter paper, 25mL polypropylene PP disappear
Xie Guan；
Sample pre-treatments：The Australia dragon design spot liver powder that 1.0g is ready for is weighed, the PP resolutions of 25mL polypropylene are placed in
5.0mL nitric acid and 2.0mL hydrogen peroxide is added in Guan Zhong, and standing is transparent to solution, and polypropylene PP digestion tubes are then placed in electricity
In heat resolution instrument, in 90 DEG C of heating resolution 1h, temperature is improved after resolution and continues to be heated to nitrogen dioxide tobacco ease to 110 DEG C
To the greatest extent, polypropylene PP digestion tubes are taken out, 1mL ammonium dihydrogen phosphates are added after cooling, polypropylene PP resolutions are diluted to distilled water
The quantitative scale of pipe, shakes up, and Australia dragon design spot liver sample is made, to be measured；
Other steps are identical as embodiment one.
Embodiment three
The present embodiment provides a kind of Cadmium detrmination method in animal's liver, the differences of the assay method and embodiment one
It is：
Animal's liver sample to be tested prepares：Pig liver dry-eye disease 400g is weighed, uniform powder is broken into grinder, and
80 mesh sieve is crossed, using quartering by above-mentioned pig liver powder division to 80g, is contained in clean, dry medicine bottle, and carry out mark
Note preserves, spare；
Instrument reagent prepares：The electric heating that temperature controlling range is 0 DEG C~300 DEG C clears up instrument, weighing accuracy to 0.0001g
Assay balance, grinder, the atomic absorption spectrophotometer with nickel light source, graphite furnace, ashless filter paper, the poly- 4- methyl-of 50mL
1- amylene digestion tubes；
Sample pre-treatments：The pig liver powder that 0.5g is ready for is weighed, the poly- 4- methyl-1s of 50mL-amylene resolution is placed in
5.0mL nitric acid and 2.0mL perchloric acid is added in Guan Zhong, and it is in water white transparency to stand to solution, then by the poly(4-methyl-1-pentene)
Digestion tube is placed in electric heating resolution instrument, in 60 DEG C of heating resolution 2h, temperature is improved after resolution and continues to be heated to two to 110 DEG C
Nitrogen oxide tobacco ease to the greatest extent, takes out the poly- 4- methyl-1s-amylene digestion tube, adds 1mL ammonium dihydrogen phosphates after cooling, use distilled water
It is diluted to the quantitative scale of the poly- 4- methyl-1s-amylene digestion tube, is shaken up, pig liver sample is made, while doing blank sample, waits for
It surveys；
Other steps are identical as embodiment one.
It is to wait for Australia dragon design spot liver specimens when assay technical solution of the present invention measures the technique effect of scheme
Sample is measured, and Fig. 1 is the cadmium standard curve drawn according to the above method, and table one is is used technical side according to the present invention
The calculated method detection limit of the step of method institute, table two is according to the step of being used technical method calculated essence of the invention
Density value, table three is according to the step of being used technical method calculated recovery of standard addition value of the invention.
One method detection limit of table
Two precision values of table
Three recovery of standard addition of table
By above-mentioned chart data it is found that the calibration curve coefficient correlation R of the technical method of the present invention2It is 0.9957, is more than
0.995；Method detection is limited to 0.012mg/kg, is less than GB5009.15-2014《The survey of national food safety standard cadmium in foods
It is fixed》Middle method detection is limited to the regulation of 0.001mg/Kg, again smaller than GB 15201-1994《Cadmium in foods tolerance limit》It is right
In the regulation of cadmium content≤0.1mg/kg in animal；Precision is 1.56%, is less than 5%；Recovery of standard addition is 92.06%
~104.06%, average recovery rate 97.22%.
When as a result proving to detect the cadmium in animal's liver with technical solution of the present invention, calibration curve coefficient correlation value is more
Height, method detection limit 0.012mg/kg, precision is more preferable, and recovery of standard addition meets the requirements.
To sum up, technical scheme of the present invention uses transparent and with a scale polyolefin digestion tube to animal's liver sample to be measured
Product are cleared up, and volumetric flask progress constant volume is transferred to without being washed to digestion tube, again by cleaning solution after resolution, but
The constant volume directly in the digestion tube, not only simplifies operating procedure, and reduces because of operating procedure and washing transfer constant volume mistake
Operating error in journey.In the sample pre-treatments of the present invention, animal's liver sample to be tested was impregnated through pernitric acid and hydrogen peroxide
Solution is just transparent after night, and it need to be 60 DEG C~90 DEG C in temperature to be placed in after electric heating resolution instrument only, and heating digestion time is 1h~2h
Just enough, with traditional in thermostatic drying chamber, 120 DEG C~160 DEG C digestion 4h~6h of temperature are compared, and reduce digestion temperature
Degree, shortens digestion time.The cadmium detected with technical solution of the present invention in animal's liver is can be seen that from testing result simultaneously
When, the calibration curve coefficient correlation value higher made, method detection limit 0.012mg/kg, precision is more preferable, recovery of standard addition
It meets the requirements, large-scale promotion can be carried out in the applications such as the safe and healthy supervision in the market of animal food to the method.
It should be noted that although the various embodiments described above have been described herein, it is not intended to limit
The scope of patent protection of the present invention.Therefore, based on the present invention innovative idea, to embodiment described herein carry out change and repair
Change, or using equivalent structure or equivalent flow shift made by description of the invention and accompanying drawing content, it directly or indirectly will be with
Upper technical solution is used in other related technical areas, is included within the scope of patent protection of the present invention.
Claims (10)
1. a kind of Cadmium detrmination method in animal's liver, which is characterized in that the assay method includes：
Animal's liver sample to be tested prepares and cadmium Specification Curve of Increasing；
Sample to be tested pre-treatment, Specimen Determination and quantitative calculating；
The sample to be tested pre-treatment step includes：
Weigh the animal's liver sample to be tested being ready for, be placed in can be read volume data and can constant volume transparent digestion container
In, strong acid and strong oxidizer is added, stands, then is placed in heat resolution instrument to heat by the digestion container and clear up, resolution terminates
After continue to be heated to tobacco ease to the greatest extent, take out the digestion container, add matrix modifier after cooling, the resolution is diluted to purified water
Container constant volume graduation mark, shakes up, and animal's liver sample is made, to be measured；
The Specimen Determination is the cadmium absorbance for measuring the animal's liver sample, described to be quantitatively calculated as animal's liver sample
The cadmium absorbance value of measurement corresponds to cadmium standard curve progress cadmium concentration and quantitatively calculates.
2. Cadmium detrmination method in animal's liver according to claim 1, which is characterized in that the digestion container is polyene
Hydro carbons digestion tube, the polyolefin include one kind or more in polyethylene, polypropylene, poly 1-butene and poly(4-methyl-1-pentene)
Kind.
3. Cadmium detrmination method in animal's liver according to claim 2, which is characterized in that the constant volume of the digestion container
Volume range is 1mL~100mL.
4. Cadmium detrmination method in animal's liver according to claim 1, which is characterized in that the heat resolution instrument is electric heating
It clears up instrument or bath clears up instrument.
5. Cadmium detrmination method in animal's liver according to claim 1, which is characterized in that the animal's liver waits for test sample
Product are that the dry-eye disease is ground into grain diameter and be less than by dry-eye disease or fresh sample if animal's liver sample to be tested is dry-eye disease
The uniform powder of 40 mesh is stored in clean container, and marks, and saves backup；If animal's liver sample to be tested is fresh
The fresh sample is then broken into homogenate by sample, is stored in clean container, and mark, is saved backup in freezing equipment.
6. Cadmium detrmination method in animal's liver according to claim 5, which is characterized in that weigh the animal's liver and wait for
It surveys powder or is homogenized 300g~600g, it is spare using quartering division to 60g~120g.
7. Cadmium detrmination method in animal's liver according to claim 1, which is characterized in that the strong acid is nitric acid, is added
It is 3.0mL~6.0mL to enter amount, and the strong oxidizer is hydrogen peroxide or perchloric acid, and addition is 1.0mL~3.0mL.
8. Cadmium detrmination method in animal's liver according to claim 7, which is characterized in that heating resolution be with
What lower condition carried out：Temperature is 60 DEG C~90 DEG C, and heating digestion time is 1h~2h, continues to be heated to titanium dioxide after resolution
Nitrogen tobacco ease is to the greatest extent.
9. Cadmium detrmination method in animal's liver according to claim 8, which is characterized in that the described matrix of addition is improved
Agent is ammonium dihydrogen phosphate, and additive amount is 0.5mL~2mL.
10. according to Cadmium detrmination method in animal's liver according to any one of claims 1 to 9, which is characterized in that the suction
Shading value measurement is carried out in the following conditions：Wavelength 228.8nm, lamp current 2mA~10mA, 105 DEG C of drying temperature, when dry
Between 20s~30s, 400 DEG C~700 DEG C, ashing time 20s~40s of ashing temperature, 1300 DEG C~2300 DEG C of atomization temperature is former
Sonization time 3s~5s.
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| Publication number | Priority date | Publication date | Assignee | Title |
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