CN110609068A - Method for rapidly extracting and detecting lead and cadmium in grains - Google Patents
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Abstract
A method for rapidly extracting and detecting lead and cadmium in grains comprises the following steps: crushing and sieving a grain sample, mixing with the extracting solution, shaking up by oscillation, and standing to obtain a sample treatment solution; adding a modifier and a masking agent into the acetic acid-sodium acetate-ammonium acetate buffer solution, uniformly mixing, and adding the sample treatment solution obtained in the step S1 to obtain a detection solution; the detection solution in step S2 is detected using a screen-printed electrode and an adsorption stripping voltammetry. The invention has the advantages of simple and quick sample pretreatment, sensitive detection, interference resistance, no need of specific expensive instruments and reagents, and capability of realizing on-site quick screening by using a portable instrument.
Description
Technical Field
The invention relates to the technical field of grain heavy metal analysis, in particular to a method for quickly extracting and detecting lead and cadmium in grains.
Background
The food quality safety is related to the national civilization. With the rapid development of industrialization in China, heavy metal pollution is more serious, and heavy metal pollutants can enter the bodies of grain crops through soil, water and the atmosphere in the planting areas of the grain crops, so that the content of heavy metal in the grains is finally over-standard. In recent years, the living standard of people is continuously improved, people pay more attention to their health, people pay more and more attention to the quality safety of grains, the health of human bodies is seriously affected by the grains with the overproof heavy metal lead and cadmium contents after being ingested for a long time, and the rapid extraction and quantitative detection of the heavy metal contents in the grains are very important through an effective method.
At present, common grain heavy metal extraction methods comprise wet digestion, microwave digestion, pressure tank digestion and the like, wherein the digestion and extraction time is long, about 2-4 hours, and even needs to stay overnight; the process is dangerous and complex, and needs concentrated nitric acid, concentrated sulfuric acid, perchloric acid, hydrogen peroxide and the like. Common methods for detecting heavy metal ions include: inductively coupled plasma mass spectrometry, atomic absorption and emission spectrometry, atomic fluorescence spectrometry, and the like. The traditional technical methods all need to rely on complex instruments and equipment in the detection process, are complicated in operation steps, need professional technicians and are not suitable for rapid field detection. Therefore, research and development of a novel grain heavy metal on-site detection method with simple operation, short detection time and high sensitivity is urgently needed.
The electrochemical detection method is one of the most classical methods for heavy metal detection, and has the advantages of high sensitivity, multiple detection types, simple detection process and the like. The glassy carbon electrode and the gold electrode are commonly used electrodes in an electrochemical detection method, have the advantages of wide potential window, low detection limit and the like, but are troublesome to maintain and use, need to be cleaned and polished before each test, and are not easy to popularize and use on a large scale. The screen printing electrode integrates the working electrode, the reference electrode and the auxiliary electrode together, is in a chip shape, is convenient to use, is easy for batch production and quality control, has commercial production advantages, and is increasingly applied to the aspect of heavy metal detection.
Disclosure of Invention
In order to solve the problems, the invention provides a method for quickly extracting and detecting lead and cadmium in grains, the pretreatment of a sample is simple and quick, the detection is sensitive, the interference resistance is realized, special expensive instruments and reagents are not needed, and the field quick screening can be realized by using a portable instrument.
The invention discloses a method for quickly extracting and detecting lead and cadmium in grains, which is characterized by comprising the following steps of:
s1, crushing and sieving the grain samples, mixing with the extracting solution, shaking up, and standing to obtain a sample treatment solution;
s2, adding a modifier and a masking agent into the acetic acid-sodium acetate-ammonium acetate buffer solution, mixing uniformly, and adding the sample treatment solution obtained in the step S1 to obtain a detection solution;
the modifier is one of bismuth, antimony or mercury, and the concentration of the modifier is 0.1-100 mg/kg;
the masking agent is one or more of sodium thiosulfate, sodium sulfite, hexamethylenetetramine, phenylthiourea, thiosemicarbazide and potassium iodide, and the concentration of the masking agent is 0.3-2.5 wt.%;
s3, detecting the detection solution in the step S2 by using a screen printing electrode and an adsorption stripping voltammetry method;
the conditions of the adsorption stripping voltammetry are as follows: the detection potential is-1 to-0.5V, the voltage increment is 4mV, the amplitude is 0.025V, the frequency is 15Hz, the enrichment potential is-1.5V, and the enrichment time is 200 s.
Further, in step S2, the ratio of acetic acid in the buffer: sodium acetate: the volume ratio of ammonium acetate is 2-4: 1-4: 2-5; in the step S2, the mass ratio of the sample treatment solution to the buffer solution is 1-3: 7 to 9.
Still further, in step S2, the ratio of acetic acid in the buffer: sodium acetate: the volume ratio of ammonium acetate is 3:4: 3; in step S2, the mass ratio of the sample treatment solution to the buffer solution is 1: 5.
still further, in step S1, the extracting solution is one of sulfuric acid, hydrochloric acid, perchloric acid or nitric acid, and the concentration of the extracting solution is 5-20 vol.%;
in the step S1, the mass ratio of the grain sample to the extracting solution is 1: 3-5;
in the step S1, the oscillation temperature and the oscillation time are respectively 10-60 ℃ and 20S-10 min;
and in the step S1, the standing time is 2-10 min.
Further, the concentration of the extracting solution in the step S1 is 9-15 vol.%;
in the step S1, the oscillation temperature and the oscillation time are respectively 15-25 ℃ and 30S-2 min;
the standing time in step S1 was 3 min.
Further, the grain samples are crushed in step S1 and screened through a 40-mesh screen.
The invention has the beneficial effects that:
according to the invention, heavy metal lead and cadmium in grains are rapidly extracted by using various acid solutions, the extraction time is only 20 seconds as short as possible, simultaneously matrix interference introduced by rapid extraction is masked by adding various masking agents such as sodium thiosulfate, sodium sulfite, hexamethylenetetramine, phenylthiourea, thiosemicarbazide or potassium iodide, the masking agents have the effects of complexing and enriching heavy metal lead or cadmium, signals can be further enhanced, and the on-site, simple, rapid and high-sensitivity detection of heavy metal lead and cadmium in grains is realized by using a portable electrochemical detector and an adsorption stripping voltammetry. The extraction and detection method provided by the invention has the most prominent characteristics that the extraction and detection of lead and cadmium in the grain sample can be completed in a very short time, the matrix interference problem is perfectly solved by introducing the masking agent, the whole test can be completed in 10 minutes at the shortest time, and meanwhile, the operation is simple and rapid, so that the method is extremely suitable for on-site and rapid screening and has good market application prospect.
Drawings
Fig. 1 is a lead calibration curve prepared using a rice flour component analysis standard substance according to the present invention.
FIG. 2 is a cadmium calibration curve prepared using a rice flour component analysis standard substance according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
(1) Taking rice flour component analysis standard substances (GBW (E)100348, Steel grinding Nake detection technology limited company), dissolving 1g of rice standard substance powder in 5g of 10 vol.% sulfuric acid, shaking by hand for 2min, standing for 3min, extracting lead ions, adding acetic acid-sodium acetate-ammonium acetate (volume ratio is 3:4:3) buffer solution, mercury nitrate (final concentration is 10mg/kg) and sodium sulfite (final concentration is 5wt. -%) into supernate according to the lead content (0.12mg/kg) marked in the rice standard substance, and preparing into lead standard solutions with lead ion concentrations of 0, 50, 130, 150, 180, 210 and 240 ppb;
(2) connecting a screen printing electrode with a portable electrochemical workstation, then placing the screen printing electrode into the lead standard solution in the step (1), and selecting a square wave voltammetry method, wherein the potential window is-1V to-0.5V, the voltage increment is 4mV, the amplitude is 0.025V, the frequency is 15Hz, the enrichment potential is-1.5V, and the enrichment time is 200 s; and recording the current value, testing the lead standard solution with each concentration for 5 times respectively, taking the mean value of 5 times to assign a lead standard curve, and obtaining the data as the following table.
Example 2
(1) Firstly, taking 100g (150ppb cadmium content) of a No. 1 rice sample, crushing by a crusher, and sieving by a 40-mesh sieve;
(2) taking 1g of a crushed and sieved rice sample, putting the crushed and sieved rice sample into a centrifugal tube, adding 5g of 10 vol.% sulfuric acid, shaking by hand for 2min, standing and standing for 3 min;
(3) taking 1mL of acetic acid-sodium acetate-ammonium acetate buffer solution with the volume ratio of 3:4:3, adding mercury nitrate with the final concentration of 10mg/kg, adding 10 mu L of 5 wt.% sodium sulfite, uniformly mixing to obtain a blank solution, adding 200 mu L of the supernatant obtained in the step (2), and uniformly mixing to obtain a mixed solution;
(4) connecting the screen printing electrode with a portable electrochemical workstation, sequentially testing the blank solution and the mixed solution in the step (3), and selecting square wave voltammetry, wherein a potential window is-1V to-0.5V, a voltage increment is 4mV, an amplitude is 0.025V, a frequency is 15Hz, an enrichment potential is-1.5V, and an enrichment time is 200 s; the detected current values were obtained, and the results of detection calculated using the lead standard curve are shown in the following table.
Blank solution detection results:
serial number | Current value (μ A) |
1 | 0.006 |
2 | 0.004 |
3 | 0.003 |
4 | 0.006 |
5 | 0.008 |
Mean value | 0.0054 |
Detection results of the mixed solution:
serial number | Current value (μ A) | Cadmium concentration (ppb) |
1 | 0.281 | 148.9 |
2 | 0.302 | 159.4 |
3 | 0.281 | 149.0 |
4 | 0.317 | 166.9 |
5 | 0.306 | 161.7 |
6 | 0.286 | 151.6 |
7 | 0.272 | 144.7 |
8 | 0.282 | 149.8 |
9 | 0.288 | 152.4 |
10 | 0.287 | 152.2 |
Mean value | 0.290 | 153.7 |
Standard deviation of | 0.013 | 6.5 |
CV | 4.5% | 4.2% |
Comparative example 2
The experimental procedure was as in example 2 except that no sodium sulfite was added and the test results are shown in the following table:
blank solution detection results:
detection results of the mixed solution:
serial number | Current value (μ A) | Cadmium concentration (ppb) |
1 | 0.381 | 198.8 |
2 | 0.452 | 234.3 |
3 | 0.441 | 228.8 |
4 | 0.517 | 266.7 |
5 | 0.506 | 261.5 |
6 | 0.420 | 218.5 |
7 | 0.391 | 204.0 |
8 | 0.372 | 194.7 |
9 | 0.411 | 213.8 |
10 | 0.443 | 230.1 |
Mean value | 0.433 | 225.1 |
Standard deviation of | 0.047 | 23.3 |
CV | 10.8% | 10.3% |
As can be seen from the test results of the blank solutions of example 2 and comparative example 2, sodium sulfite masks the current reaction in the blank solution, and at the same time, Hg+The oxidation potential is 0.5V, so that the background component masked by sodium sulfite here is not Hg+. From the test results of the mixed solutions of example 2 and comparative example 2, it can be seen that the mean value of the current values of the solution containing no sodium sulfite was higher by 49.3% than that of the solution obtained by adding sodium sulfite, while the standard deviation of the test results of the solution was lower and the test was more stable after adding sodium sulfite.
Example 3
(1) Taking rice flour component analysis standard substances (GBW (E)100348, Steel grinding Nake detection technology limited company), dissolving 1g of rice standard substance powder with 5g of 10 vol.% hydrochloric acid, shaking by hand for 2min, standing for 5min, extracting cadmium ions, adding acetic acid-sodium acetate-ammonium acetate (volume ratio of 3:4:3) buffer solution, bismuth nitrate (final concentration of 1mg/kg) and potassium iodide (final concentration of 5 wt.% per thousand) into the supernatant according to the cadmium content (0.24mg/kg) identified in the rice standard substance, and preparing standard solutions with the cadmium ion concentrations of 50, 130, 150, 180, 210 and 240 ppb;
(2) connecting a screen printing electrode with a portable electrochemical workstation, then placing the screen printing electrode into the lead standard solution in the step (1), and selecting a square wave voltammetry method, wherein the potential window is-1V to-0.5V, the voltage increment is 4mV, the amplitude is 0.025V, the frequency is 15Hz, the enrichment potential is-1.5V, and the enrichment time is 200 s; and recording the current value, respectively testing 5 times by using the cadmium standard solution with each concentration, taking the mean value of 5 times to designate a cadmium standard curve, and obtaining the data as shown in the following table.
Example 4
(1) Firstly, taking 100g of a No. 1 sample (with the cadmium content of 250 ppb) of the brown rice, crushing by a crusher, and sieving by a 40-mesh sieve.
(2) Taking 1g of the crushed and sieved rice sample, putting the crushed and sieved rice sample into a centrifugal tube, adding 5g of 10% hydrochloric acid, shaking by hand for 2min, standing and standing for 5 min.
(3) Taking 1mL of acetic acid-sodium acetate-ammonium acetate buffer solution with the volume ratio of 3:4:3, adding 1mg/kg of bismuth nitrate with the final concentration, adding 10 mu L of 5% potassium iodide, uniformly mixing to obtain a blank solution, adding 200 mu L of the supernatant obtained in the step (2), and uniformly mixing to obtain a mixed solution.
(4) After connecting the screen printing electrode with a portable electrochemical workstation, respectively detecting the blank capacity of the moon and the mixed solution in the step (3), and selecting square wave voltammetry, wherein a potential window is-1V to-0.5V, a voltage increment is 4mV, an amplitude is 0.025V, a frequency is 15Hz, an enrichment potential is-1.5V, and an enrichment time is 200 s; and obtaining a detection current value, and calculating according to a cadmium standard curve to obtain a detection result, wherein the detection result is shown in the following table.
Blank solution detection results:
serial number | Current value (μ A) |
1 | 0.004 |
2 | 0.006 |
3 | 0.003 |
4 | 0.006 |
5 | 0.004 |
Mean value | 0.0046 |
Detection results of the mixed solution:
serial number | Current value (μ A) | Cadmium concentration (ppb) |
1 | 0.499 | 258.0 |
2 | 0.487 | 251.8 |
3 | 0.482 | 249.5 |
4 | 0.492 | 254.3 |
5 | 0.448 | 232.6 |
6 | 0.526 | 271.6 |
7 | 0.481 | 249.1 |
8 | 0.539 | 277.8 |
9 | 0.543 | 279.8 |
10 | 0.411 | 213.9 |
Mean value | 0.491 | 253.8 |
Standard deviation of | 0.038 | 19.1 |
CV | 7.8% | 7.5% |
Comparative example 4
The procedure is as in example 2 except that potassium iodide is not added. The results are shown in the following table:
blank solution detection results:
detection results of the mixed solution:
serial number | Current value (uA) | Cadmium concentration (ppb) |
1 | 0.549 | 282.9 |
2 | 0.637 | 326.6 |
3 | 0.642 | 329.4 |
4 | 0.692 | 354.1 |
5 | 0.668 | 342.4 |
6 | 0.660 | 338.4 |
7 | 0.600 | 308.4 |
8 | 0.629 | 322.7 |
9 | 0.696 | 356.1 |
10 | 0.521 | 268.8 |
Mean value | 0.629 | 323.0 |
Standard deviation of | 0.055 | 27.4 |
CV | 8.7% | 8.5% |
As can be seen from the test results of the blank solutions of example 4 and comparative example 4, potassium iodide masks the galvanic reaction in the blank solution in consideration of Ag+Has an oxidation potential of 0.1V, where the background substance masked by potassium iodide is not Ag+. From the test results of the mixed solutions of example 4 and comparative example 4, it can be seen that the average value of the current values of the solutions not containing potassium iodide was higher by 28.1% than that of the solution obtained by adding potassium iodide.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (6)
1. A method for rapidly extracting and detecting lead and cadmium in grains is characterized by comprising the following steps:
s1, crushing and sieving the grain samples, mixing with the extracting solution, shaking up, and standing to obtain a sample treatment solution;
s2, adding a modifier and a masking agent into the acetic acid-sodium acetate-ammonium acetate buffer solution, mixing uniformly, and adding the sample treatment solution obtained in the step S1 to obtain a detection solution;
the modifier is one of bismuth, antimony or mercury, and the concentration of the modifier is 0.1-100 mg/kg;
the masking agent is one or more of sodium thiosulfate, sodium sulfite, hexamethylenetetramine, phenylthiourea, thiosemicarbazide and potassium iodide, and the concentration of the masking agent is 0.3-2.5 wt.%;
s3, detecting the detection solution in the step S2 by using a screen printing electrode and an adsorption stripping voltammetry method;
the conditions of the adsorption stripping voltammetry are as follows: the detection potential is-1 to-0.5V, the voltage increment is 4mV, the amplitude is 0.025V, the frequency is 15Hz, the enrichment potential is-1.5V, and the enrichment time is 200 s.
2. The method for rapidly extracting and detecting lead and cadmium in grains according to claim 1, which is characterized in that:
acetic acid in buffer described in step S2: sodium acetate: the volume ratio of ammonium acetate is 2-4: 1-4: 2-5; in the step S2, the mass ratio of the sample treatment solution to the buffer solution is 1-3: 7 to 9.
3. The method for rapidly extracting and detecting lead and cadmium in grains according to claim 1 or 2, which is characterized in that: acetic acid in buffer described in step S2: sodium acetate: the volume ratio of ammonium acetate is 3:4: 3; in step S2, the mass ratio of the sample treatment solution to the buffer solution is 1: 5.
4. the method for rapidly extracting and detecting lead and cadmium in grains according to claim 1, which is characterized in that:
in the step S1, the extracting solution is one of sulfuric acid, hydrochloric acid, perchloric acid or nitric acid, and the concentration of the extracting solution is 5-20 vol.%;
in the step S1, the mass ratio of the grain sample to the extracting solution is 1: 3-5;
in the step S1, the oscillation temperature and the oscillation time are respectively 10-60 ℃ and 20S-10 min;
and in the step S1, the standing time is 2-10 min.
5. The method for rapidly extracting and detecting lead and cadmium in grains according to claim 1, which is characterized in that:
the concentration of the extracting solution in the step S1 is 9-15 vol.%;
in the step S1, the oscillation temperature and the oscillation time are respectively 15-25 ℃ and 30S-2 min;
the standing time in step S1 was 3 min.
6. The method for rapidly extracting and detecting lead and cadmium in grains according to claim 1, which is characterized in that: and step S1, crushing the grain sample and sieving the crushed grain sample with a 40-mesh sieve.
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CN115201289A (en) * | 2021-04-12 | 2022-10-18 | 广东朗源生物科技有限公司 | Heavy metal detection method based on screen printing electrode and detection instrument thereof |
CN113218727A (en) * | 2021-04-30 | 2021-08-06 | 北京美正生物科技有限公司 | Pretreatment method for quickly extracting lead and cadmium in grain sample |
CN114216949A (en) * | 2021-11-18 | 2022-03-22 | 佛山科学技术学院 | Screen printing electrode, manufacturing method and detection method thereof |
CN114216949B (en) * | 2021-11-18 | 2023-08-08 | 佛山科学技术学院 | Screen printing electrode, manufacturing method and detection method thereof |
CN114563572A (en) * | 2022-04-27 | 2022-05-31 | 成都安普诺生物科技有限公司 | Tobacco leaf all-in-one heavy metal rapid quantitative detection card and detection method |
CN114563572B (en) * | 2022-04-27 | 2022-08-02 | 成都安普诺生物科技有限公司 | Tobacco leaf all-in-one heavy metal rapid quantitative detection card and detection method |
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