CN117969644A - Method for determining uranium content in biological sample by microwave digestion ICP-MS method - Google Patents
Method for determining uranium content in biological sample by microwave digestion ICP-MS method Download PDFInfo
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- CN117969644A CN117969644A CN202311849215.6A CN202311849215A CN117969644A CN 117969644 A CN117969644 A CN 117969644A CN 202311849215 A CN202311849215 A CN 202311849215A CN 117969644 A CN117969644 A CN 117969644A
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 37
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000012472 biological sample Substances 0.000 title claims abstract description 30
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract description 29
- 238000000120 microwave digestion Methods 0.000 title claims abstract description 22
- 230000029087 digestion Effects 0.000 claims abstract description 23
- 239000000523 sample Substances 0.000 claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 210000000056 organ Anatomy 0.000 claims abstract description 12
- 241001465754 Metazoa Species 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 2
- 210000001519 tissue Anatomy 0.000 description 6
- 238000002203 pretreatment Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000002372 labelling Methods 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 238000000184 acid digestion Methods 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007619 statistical method Methods 0.000 description 2
- 238000012313 Kruskal-Wallis test Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The invention belongs to the technical field of biological detection, and relates to a method for measuring uranium content in a biological sample by a microwave digestion ICP-MS method. The method comprises the following steps: (1) weighing a quantity of animal tissue or organ; (2) Placing the weighed animal tissues or organs into a reaction tank, and adding concentrated nitric acid solution to perform pre-digestion; (3) Transferring the pre-digested sample to a rotor, and assembling the rotor to a digestion instrument for microwave digestion; (4) After digestion is completed, the reaction tank is taken out and placed on an acid-dispelling plate for acid-dispelling operation; (5) after acid removal, transferring and fixing the volume; (6) carrying out ICP-MS on-line detection on the prepared solution; and (7) calculating uranium content. The method for measuring the uranium content in the biological sample by using the microwave digestion ICP-MS method has the advantages of simple operation steps, high analysis and test efficiency, high recovery rate, low detection limit, relatively fewer used reagents and environmental friendliness and personnel friendliness.
Description
Technical Field
The invention belongs to the technical field of biological detection, and particularly relates to a method for measuring uranium content in a biological sample by a microwave digestion ICP-MS method.
Background
Uranium (U) is widely used in nuclear industry and military operations as a strategic resource for defense industry and nuclear power industry. During the production and use of uranium, the uranium is inevitably released into the environment, then enters the human body through the respiratory tract, the digestive tract or the skin, and is distributed into organs such as the kidney, the bone and the liver, and radiation damage and chemical damage are caused to the human body. Therefore, the uranium content of the biological sample is detected, and the distribution condition of uranium in each organ tissue after the uranium enters the organism can be known.
ICP-MS, collectively known as inductively coupled plasma-mass spectrometry (Inductively coupled plasma-Mass Spectrometry), is an analytical instrument that combines ICP technology with mass spectrometry technology. The ICP-MS method has the advantages of simple sample preparation and sample injection technology, high mass scanning speed, short operation period, small interference degree of provided ion information and the like. For most elements, there is a very low detection limit, and it is recognized as the most ideal inorganic element analysis method. In addition, the ICP-MS method can analyze almost all metal elements in the periodic table, the detection limit is below 1ppt, and meanwhile, the ICP-MS method can also analyze most nonmetallic elements.
The prior pretreatment method for measuring the uranium content in the biological sample comprises a pretreatment method (HJ 840-2017) of analyzing trace uranium in an environmental sample, wherein the biological sample is pretreated by drying, carbonizing, ashing and electric hot plate acid digestion.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for measuring the uranium content in a biological sample by a microwave digestion ICP-MS method. The method has the advantages of high digestion speed, high digestion rate, relatively few reagents, and environmental friendliness and personnel friendliness.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
A method for determining uranium content in a biological sample by a microwave digestion ICP-MS method comprises the following steps:
(1) Weighing a certain amount of animal tissues or organs;
(2) Placing the weighed animal tissues or organs into a reaction tank, and adding concentrated nitric acid solution to perform pre-digestion;
(3) Transferring the pre-digested sample to a rotor, and assembling the rotor to a digestion instrument for microwave digestion;
(4) After digestion is completed, the reaction tank is taken out and placed on an acid-dispelling plate for acid-dispelling operation;
(5) After the acid removal is finished, transferring and fixing the volume;
(6) Performing ICP-MS on-line detection on the prepared solution;
(7) And calculating uranium content.
Further, in the step (1), 0.1 to 0.3g of the animal tissue or organ is weighed.
Further, in the step (2), the mass fraction of the concentrated nitric acid is 68%, the adding amount is 3mL, and the pre-digestion condition is 130 ℃ for 20min.
Further, in the step (3), the reaction conditions are: heating to 120deg.C from room temperature for 5min, maintaining for 5min, heating to 180deg.C at 12deg.C/min, maintaining for 10min, and cooling to 55deg.C.
Further, in the step (4), the acid-expelling heating temperature is 160 ℃.
In the step (5), the acid in the reaction tank is driven to leave a small drop of liquid, the small drop of liquid is transferred to a 10mL centrifuge tube by using acidified water with pH of 2, the volume is fixed to 4-6 mL, and then ultrapure water is used for fixing the volume to the scale.
In step (6), if the detection exceeds the linear range, the detection is performed after dilution with ultrapure water.
Further, in step (7), the uranium content is calculated as follows:
Wherein: c-uranium concentration in sample, μg/g;
C1-determining the concentration of the sample in the solution, μg/L;
k is dilution multiple, and the sample is used when dilution measurement is needed;
10-constant volume after digestion of sample, mL;
m1-weigh biological sample weight, g.
The invention has the beneficial effects that: the method for determining the uranium content in the biological sample by using the microwave digestion ICP-MS method has the advantages of high digestion speed, high digestion rate, relatively fewer reagents and environmental friendliness and personnel friendliness.
Detailed Description
The practice of the invention is further illustrated by the following examples, but the embodiments of the invention are not limited to the following examples.
Example 1:
1. Experimental procedure
1.1 Sample weighing
About 0.1 to 0.3g of animal tissue or organ is weighed, and M1 is weighed.
1.2 Digestion
(1) Placing the weighed animal tissues or organs into a reaction tank, adding 3mL of concentrated nitric acid with the mass fraction of 68%, and carrying out pre-digestion on an acid-expelling plate at 130 ℃ for 20min;
(2) Transferring the pre-digested sample to a rotor, and assembling the sample to a digestion instrument;
(3) The reaction conditions are set as follows: heating to 120deg.C from room temperature for 5min, maintaining for 5min, heating to 180deg.C at 12deg.C/min, maintaining for 10min, and cooling to 55deg.C;
(4) After the digestion procedure is completed, taking out the reaction tank, placing the reaction tank in an acid-dispelling plate, and performing acid-dispelling operation at 160 ℃;
(5) Acid is removed from the reaction tank until a small drop of liquid is left, acidified water with the pH value of 2 is transferred to a 10mL centrifuge tube, after the constant volume is 4-6 mL, ultrapure water is used for constant volume to scale;
1.3 uranium content determination
And (3) performing ICP-MS on-line detection on the digested biological sample, and if the digested biological sample exceeds the linear range, diluting the digested biological sample with ultrapure water and performing detection.
1.4 Calculation of results
The uranium content in the biological sample is calculated as follows:
Wherein: c-uranium concentration in sample, μg/g;
C1-determining the concentration of the sample in the solution, μg/L;
K-dilution fold (for samples requiring dilution measurement);
10-constant volume after digestion of sample, mL;
m1-weigh biological sample weight, g.
2. Statistical analysis
SPSS22.0 statistical software is adopted to carry out statistical analysis on the same biological sample subjected to ashing, electric hot plate acid digestion and microwave digestion, and according to whether normal distribution is met, variance analysis or Kruskal-Wallis test (non-normal) is used for comparison among groups, and P is less than or equal to 0.05 and has statistical significance for difference.
3. Analysis of results
(1) Comparison experiment
By performing ICP-MS detection on samples treated by the two methods, the results show that the detection results have no statistical significance (P is more than 0.05), which indicates that the microwave digestion ICP-MS method can be used for pretreatment of the samples. See table 1.
Table 1 comparison of the results of the different pretreatment methods (n=3)
(2) Accuracy of
The marking experiment is carried out by adopting different pretreatment methods on the same sample: the same sample is uniformly divided into two equal parts, one part is subjected to pretreatment on-machine measurement, and the other part is added with a certain amount of uranium standard solution and then subjected to pretreatment on-machine measurement. The calculated recovery rate of the electric heating plate disinfection method for labeling is 90.3-106.2%, and the recovery rate of the microwave disinfection method for labeling is 92.2-103.5%, which shows that the recovery rate of the microwave disinfection method for labeling is higher and the accuracy is better. See table 2.
TABLE 2 comparison of detection result accuracy for different pretreatment methods
The result shows that the digestion rate of the biological sample digested by the microwaves is higher, and the treatment effect of the sample is better.
According to the embodiment, the method for determining the uranium content in the biological sample by using the microwave digestion ICP-MS method effectively shortens the pretreatment time and flow, has the advantages of simple operation steps, high analysis and test efficiency, high recovery rate, low detection limit of the method, relatively fewer reagents, environmental friendliness and personnel friendliness, and realizes rapid and accurate analysis of the uranium content of the biological sample.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof. The foregoing examples or embodiments are merely illustrative of the invention, which may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims are intended to be encompassed within the scope of the invention.
Claims (8)
1. The method for measuring the uranium content in the biological sample by using the microwave digestion ICP-MS method is characterized by comprising the following steps of:
(1) Weighing a certain amount of animal tissues or organs;
(2) Placing the weighed animal tissues or organs into a reaction tank, and adding concentrated nitric acid solution to perform pre-digestion;
(3) Transferring the pre-digested sample to a rotor, and assembling the rotor to a digestion instrument for microwave digestion;
(4) After digestion is completed, the reaction tank is taken out and placed on an acid-dispelling plate for acid-dispelling operation;
(5) After the acid removal is finished, transferring and fixing the volume;
(6) Performing ICP-MS on-line detection on the prepared solution;
(7) And calculating uranium content.
2. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (1), 0.1 to 0.3g of animal tissues or organs are weighed.
3. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (2), the mass fraction of the concentrated nitric acid is 68%, the adding amount is 3mL, and the pre-digestion condition is 130 ℃ for 20min.
4. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (3), the reaction conditions are as follows: heating to 120deg.C from room temperature for 5min, maintaining for 5min, heating to 180deg.C at 12deg.C/min, maintaining for 10min, and cooling to 55deg.C.
5. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (4), the acid-expelling heating temperature is 160 ℃.
6. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (5), acid in the reaction tank is driven until a small drop of liquid is left, the small drop of liquid is transferred to a 10mL centrifuge tube by acidified water with pH of 2, the volume is fixed to 4-6 mL, and then ultrapure water is used for fixing the volume to the scale.
7. The method for determining the uranium content in a biological sample by using a microwave digestion ICP-MS method according to claim 1, wherein the method comprises the following steps: in the step (6), if the detection of the upper machine exceeds the linear range, the detection is carried out after the dilution with ultrapure water.
8. A method for determining the uranium content of a biological sample by a microwave digestion ICP-MS method according to any one of claims 1 to 7, wherein: in the step (7), the uranium content is calculated according to the following formula:
Wherein: c-uranium concentration in sample, μg/g;
C1-determining the concentration of the sample in the solution, μg/L;
k is dilution multiple, and the sample is used when dilution measurement is needed;
10-constant volume after digestion of sample, mL;
m1-weigh biological sample weight, g.
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