CN109001138A - The detection method of potassium content in high potassium food - Google Patents
The detection method of potassium content in high potassium food Download PDFInfo
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- CN109001138A CN109001138A CN201811124569.3A CN201811124569A CN109001138A CN 109001138 A CN109001138 A CN 109001138A CN 201811124569 A CN201811124569 A CN 201811124569A CN 109001138 A CN109001138 A CN 109001138A
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- G—PHYSICS
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- 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
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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Abstract
The present invention relates to a kind of detection methods of potassium content in high potassium food, belong to technical field of food detection.Detection method includes the following steps: sample pre-treatments for this: taking sample to be tested, is placed in micro-wave digestion inner canister, nitric acid is added, is placed in microwave dissolver and is cleared up, catch up with acid, constant volume obtains sample solution；The configuration of standard curve: using potassium single element standard substance solution, prepares series standard curve solution；Upper machine testing: sample solution obtained above and series standard curve solution are detected with flame atomic absorption spectrophotometer, and using 404.4 ± 2nm as measurement spectral line, detect, potassium content in sample is calculated.The detection method selects 404.4 ± 2nm as measurement spectral line, for the food of high potassium content, can without dilution or dilute it is less detected, have the advantages that simple, fast.Sample recovery of standard addition is verified using national standard reference substance, is as a result satisfied between 95%~105%.
Description
Technical field
The present invention relates to technical field of food detection, more particularly to a kind of detection method of potassium content in high potassium food.
Background technique
Potassium (K) is one of important element involved in geochemistry and life process, there is important work in many fields
With, such as soil analysis, human medical, agrochemical, pharmaceuticals industry.It is generally necessary to the content of the element is precisely measured out,
Most industries are measured using atomic absorption spectrophotometer (AAS) and flame photometer (FP) at present.
It is provided according to China " measurement of potassium, sodium in GB 5009.91-2017 national food safety standard food ", with flame
Atomic absorption spectrography (AAS) measures the content of the potassium and sodium element in various food as the first method.It is possible thereby to see, NITRATE BY FLAME ATOMIC
Important function of the absorption spectrophotometer in the detection of China's modern food.And high-content potassium member is frequently encountered in actual operation
The sample of element, needing to dilute high magnification numbe could complete to measure, and may introduce large error, need to carry out method point with regard to this situation
The improvement of analysis.
Summary of the invention
Based on this, it is necessary in view of the above-mentioned problems, a kind of detection method of potassium content in high potassium food is provided, using the inspection
Survey method, for the food of high potassium content, can without dilution or dilute it is less detected, have the advantages that simple, fast.
The detection method of potassium content in a kind of high potassium food, comprising the following steps:
Sample pre-treatments: taking sample to be tested, is placed in micro-wave diminishing pot, and nitric acid is added, is placed in microwave dissolver and carries out
Resolution, catches up with acid, constant volume obtains sample solution；
The configuration of standard curve: using potassium single element standard substance solution, prepares series standard curve solution；
Upper machine testing: by sample solution obtained above and series standard curve solution with flame atomic adsorption spectrophotometry
Meter is detected, and using 404.4 ± 2nm as measurement spectral line, detects, potassium content in sample is calculated.
The detection method of potassium content in above-mentioned high potassium food, using in Flame Atomic Absorption Spectrometry Determination food when potassium,
High-content sample, which needs to dilute more multiple when wavelength 766.5nm is measured, could complete to measure, and measure in wavelength 404.4nm
When, then without diluting or diluting less.
In one of the embodiments, in the sample pre-treatments step, the sample to be tested include: nutrition fortifier,
Formula milk, pressed candy, pickled product.Above-mentioned detection method can operate with detection nutrition fortifier, formula milk, pickled product
In contour potassium food.
In one of the embodiments, in the sample pre-treatments step, according to 1g sample to be tested: 1-120mL sample is molten
The amount of liquid carries out pre-treatment and dilution.Above-mentioned detection method, it is less without diluting or diluting, have the advantages that easy to operate.
In one of the embodiments, in the sample pre-treatments step, add according to 10-15ml nitric acid/1g sample amount
Enter nitric acid and carries out micro-wave digestion.
It is stated in sample pre-treatments step in one of the embodiments, carries out micro-wave digestion method particularly includes: nitre is added
After acid, first covers and place 1-12h, be placed in microwave dissolver, 10min is warming up to 130 DEG C and 5min, 10min is kept to be warming up to
165 DEG C, subsequent 15min is warming up to 190 DEG C and 20min is kept to be cleared up, and is subsequently placed on graphite digestion furnace, in 110-140
Acid DEG C is caught up with water constant volume, to mix spare to close dry.Micro-wave digestion is carried out in the above described manner, and there is preferable resolution effect.
In one of the embodiments, in the configuration step of the standard curve, potassium in the series standard curve solution
Concentration is 0-100mg/L.Above-mentioned detection method, the range of linearity is wide, has the advantages that detection is easy.
In one of the embodiments, in the series standard curve solution potassium concn be respectively 0,10,20,50,80,
100mg/L。
In one of the embodiments, in the upper machine testing step, detected using potassium cathode modulation.
In one of the embodiments, when the detection of the flame atomic absorption spectrophotometer, the air acetylene of use
Ratio are as follows: 3-5:1；Sample lifting capacity are as follows: 5-7mL/min；Burn grease head highness are as follows: 7-8mm.Preferably, the air acetylene of use
Ratio are as follows: 4:1；Sample lifting capacity are as follows: 6mL/min；Burn grease head highness are as follows: 7.5mm.
Using 404.4 ± 2nm as measurement spectral line, since sensitivity is lower, by air acetylene ratio, sample lifting capacity with
And burning grease head highness is adjusted to above range, and signal strength can be improved.
In one of the embodiments, when the detection of the flame atomic absorption spectrophotometer, Parameter Conditions are as follows: narrow
Slit width degree: 1.2-1.4nm；Lamp current: 3.8-4.2mA；Photomultiplier tube negative high voltage 370-390V.Preferably, slit width:
1.3nm；Lamp current: 4.0mA；Photomultiplier tube negative high voltage 380V.It is detected with above-mentioned Parameter Conditions, there is preferable detection
Effect.
Compared with prior art, the invention has the following advantages:
The detection method of potassium content in a kind of high potassium food of the invention is selected 404.4 ± 2nm as measurement spectral line, is adopted
With the detection method, for the food of high potassium content, can without dilution or dilute it is less detected, have easy, fast
The advantages of.Sample recovery of standard addition between 95%~105%, using national standard reference substance carrot (GBW10047) and
Celery (GBW10048) is verified, and is as a result satisfied with.
Detailed description of the invention
Fig. 1 is the linear relationship chart of the potassium of 1 medium wavelength 766.5nm of embodiment detection；
Fig. 2 is the linear relationship chart of the potassium of 1 medium wavelength 404.4nm of embodiment detection.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give presently preferred embodiments of the present invention.But the invention can be realized in many different forms, however it is not limited to this paper institute
The embodiment of description.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more thorough
Comprehensively.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Following embodiment agents useful for same and instrument are as follows:
HITACHI Z-2010 atomic absorption spectrophotometer, using potassium cathode modulation, measure spectral line be 766.5nm and
404.4nm；
Milestone microwave dissolver；
Mi Libo ultrapure water machine IQ7000；
Graphite clears up instrument；
Nitric acid: AR grades, Merck；
In potassium single element solution reference material GSB 04-1733-2004, national non-ferrous metal and electronic material analysis test
The heart.Dilution configuration step by step again when use.
Embodiment 1
The detection method of potassium content in a kind of high potassium food, comprising the following steps:
One, the foundation of detection method.
1, sample pre-treatments.
0.5000g sample is weighed, is placed in micro-wave digestion inner canister, 6mL nitric acid is added, covers and places 1h or stay overnight, screw
Outer cover simultaneously loads onto outer tank, is placed in microwave dissolver and is cleared up.Inner canister is taken out after cooling, is placed on graphite digestion furnace, in 120
Acid DEG C is caught up with to be settled to 50mL with ultrapure water, mix spare to close dry.Blank test is done simultaneously.
Such as through detecting the curve upper limit that is above standard, then detected again after being diluted to sample solution.
2, the configuration of standard curve.
The use of potassium single element solution reference material (1000mg/L) dilution configuration concentration is respectively 0,0.1,0.5,1.0,
1.5,2.0mg/L and 0,10,20,50,80, drafting of the two groups of potassium standard solution of 100mg/L for standard curve.
3, upper machine testing.
Sample solution obtained above and series standard curve solution are examined with flame atomic absorption spectrophotometer
It surveys, and is detected according to parameters described below condition using 404.4nm and 766.5nm as measurement spectral line respectively, sample is calculated
Middle potassium content.
Air acetylene ratio: 4:1；
Sample lifting capacity: 6mL/min；
Burn grease head highness: 7.5mm；
Slit width: 1.3nm；
Lamp current: 4.0mA；
Photomultiplier tube negative high voltage: 380V.
Two, methodology validation.
1, standard curve.
According to above-mentioned detection method, selects wavelength 766.5nm to measure low concentration standard solution, draws its standard curve,
As shown in Figure 1.
According to above-mentioned detection method, selects wavelength 404.4nm to measure high standard solution, draws its standard curve,
As shown in Figure 2.
The range of linearity of 766.5nm wavelength is in 0~2.0mg/L, coefficient R it can be seen from the comparison of Fig. 1 and Fig. 2
It is 0.9994, but need to carry out appropriate or even multiple dilute when measurement high-content potassium to go up machine measurement.404.4nm the line of wavelength
For property range in 0~100mg/L, coefficient R 0.9999 can satisfy the measurement of high-content potassium.
2, the comparison of recovery of standard addition.
Measured respectively with two different wavelength sample (pressed candy), obtain 7 groups of data, the potassium content of sample compared with
It is high.Seen from table 1, two wavelength determine the potassium content come and are deviated, but in 10% error range.
The content of 1 different wave length of table measurement potassium
For the accuracy for verifying the sample, three horizontal mark-on tests are carried out, are closed by sample size with 0.5,1 and 2 multiple
System carrys out mark-on, and is confirmed according to detection method in " GB/T 27404-2008 Good Laboratory controls specification food Physico-chemical tests "
Technical requirements, rate of recovery range is related with tested constituent content, be greater than 100mg/kg, rate of recovery range is 95~105%.
The mark-on reclaims of 2 wavelength 766.5nm potassium of table
The mark-on reclaims of 3 wavelength 404.4nm potassium of table
By table 2 and table 3 as it can be seen that the rate of recovery of three horizontal mark-on tests meets in 97.7~103% and 97.6~101%
Technical requirements.
3, standard substance is verified
In order to further verify the accuracy and reliability of wavelength 404.4nm measuring method, national standard reference object is selected
Matter carrot (GBW10047) and celery (GBW10048) pre-treatment under conditions selected, measured value and recommendation compare, potassium member
The measured value of element is within the scope of recommendation, it is seen that the method measurement result is accurate and reliable.Standard substance measurement result is shown in Table 4.
4 national standard substance-measuring result of table
The method of high-content potassium compares in the different wave length measurement food of above-mentioned i interpretation of result Flame Atomic Absorption Spectrometry, tries
Test the result shows that, be measured using 404.4nm wavelength, no matter in linear relationship, precision, accuracy and reliability,
It is all similar to wavelength 766.5nm measurement result.
But the standard curve range of linearity of 404.4nm is big, during measuring high-content potassium, can be effectively controlled more
Secondary dilution bring error and repeatedly dilution wasted time.The improvement of this method is easy, quick, and can be reduced dilution and miss
Difference also ensures that the accuracy of high-content potassium measurement.
Embodiment 2
The detection method of potassium content in a kind of high potassium food selects 404.4nm as measurement spectral line, referring to embodiment 1
Method is detected, and difference is only that, in selected flame atomic absorption spectrophotometer Parameter Conditions, air acetylene ratio
Example are as follows: 4:1, sample lifting capacity are as follows: 6mL/min, burn grease head highness are as follows: 12.5mm.
Testing result shows that when measuring standard curve, absorbance is low and non-linear, not can be carried out the test of next step.
Embodiment 3
The detection method of potassium content in a kind of high potassium food selects 404.4nm as measurement spectral line, referring to embodiment 1
Method is detected, and difference is only that, in selected flame atomic absorption spectrophotometer Parameter Conditions, air acetylene ratio
Example are as follows: 1:1, sample lifting capacity are as follows: 6mL/min, burn grease head highness are as follows: 7.5mm.
Testing result shows that when measuring standard curve, absorbance is low and non-linear, not can be carried out the test of next step.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the detection method of potassium content in a kind of high potassium food, which comprises the following steps:
Sample pre-treatments: taking sample to be tested, is placed in micro-wave diminishing pot, and nitric acid is added, is placed in microwave dissolver and is cleared up,
Acid is caught up with, constant volume obtains sample solution；
The configuration of standard curve: using potassium single element standard substance solution, prepares series standard curve solution；
Upper machine testing: by sample solution obtained above and series standard curve solution with flame atomic absorption spectrophotometer into
Row detection, and using 404.4 ± 2nm as measurement spectral line, it detects, potassium content in sample is calculated.
2. the detection method of potassium content in high potassium food according to claim 1, which is characterized in that the sample pre-treatments
In step, the sample to be tested includes: nutrition fortifier, formula milk, pressed candy, pickled product.
3. the detection method of potassium content in high potassium food according to claim 1, which is characterized in that the sample pre-treatments
In step, according to 1g sample to be tested: the amount of 1-120mL sample solution carries out pre-treatment and dilution.
4. the detection method of potassium content in high potassium food according to claim 3, which is characterized in that the sample pre-treatments
In step, nitric acid is added according to 10-15ml nitric acid/1g sample amount and carries out micro-wave digestion.
5. the detection method of potassium content in high potassium food according to claim 4, which is characterized in that state sample pre-treatments step
In rapid, micro-wave digestion is carried out method particularly includes: after nitric acid is added, first covers and place 1-12h, be placed in microwave dissolver,
10min is warming up to 130 DEG C and 5min, 10min is kept to be warming up to 165 DEG C, subsequent 15min be warming up to 190 DEG C and keep 20min into
Row resolution, is subsequently placed on graphite digestion furnace, and acid is caught up with to do to close in 110-140 DEG C, with water constant volume, mixes spare.
6. the detection method of potassium content in high potassium food according to claim 1, which is characterized in that the standard curve
In configuration step, potassium concn is 0-100mg/L in the series standard curve solution.
7. the detection method of potassium content in high potassium food according to claim 6, which is characterized in that the series standard is bent
Potassium concn is respectively 0,10,20,50,80,100mg/L in line solution.
8. the detection method of potassium content in high potassium food according to claim 1-7, which is characterized in that on described
In machine testing step, detected using potassium cathode modulation.
9. the detection method of potassium content in high potassium food according to claim 8, which is characterized in that the NITRATE BY FLAME ATOMIC is inhaled
When the photometric detection of contracture light, the air acetylene ratio of use are as follows: 3-5:1；
Sample lifting capacity are as follows: 5-7mL/min；
Burn grease head highness are as follows: 7-8mm.
10. the detection method of potassium content in high potassium food according to claim 1, which is characterized in that the NITRATE BY FLAME ATOMIC
When the detection of absorption spectrophotometer, Parameter Conditions are as follows: slit width: 1.2-1.4nm；Lamp current: 3.8-4.2mA；Photoelectricity
Multiplier tube negative high voltage 370-390V.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110553899A (en) * | 2019-10-10 | 2019-12-10 | 中国石油化工股份有限公司 | Method for measuring content of arsenic element in industrial sulfur |
| CN113406026A (en) * | 2021-06-15 | 2021-09-17 | 河北冀衡赛瑞化工有限公司 | Method for measuring content of potassium oxide in fertilizer by using flame atomic absorption spectrometer |
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| CN104964939A (en) * | 2015-06-30 | 2015-10-07 | 山东丹红制药有限公司 | Method for detecting content of sodium and potassium ions in Danhong injection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110553899A (en) * | 2019-10-10 | 2019-12-10 | 中国石油化工股份有限公司 | Method for measuring content of arsenic element in industrial sulfur |
| CN113406026A (en) * | 2021-06-15 | 2021-09-17 | 河北冀衡赛瑞化工有限公司 | Method for measuring content of potassium oxide in fertilizer by using flame atomic absorption spectrometer |
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