CN114414509B - Method for detecting heavy metal chromium in food - Google Patents
Method for detecting heavy metal chromium in food Download PDFInfo
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- CN114414509B CN114414509B CN202111665035.3A CN202111665035A CN114414509B CN 114414509 B CN114414509 B CN 114414509B CN 202111665035 A CN202111665035 A CN 202111665035A CN 114414509 B CN114414509 B CN 114414509B
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 68
- 239000011651 chromium Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 32
- 235000013305 food Nutrition 0.000 title claims abstract description 29
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 56
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011259 mixed solution Substances 0.000 claims abstract description 27
- 239000000706 filtrate Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 239000002608 ionic liquid Substances 0.000 claims abstract description 12
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 235000021055 solid food Nutrition 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 8
- 230000001678 irradiating effect Effects 0.000 claims description 7
- -1 1-benzyl acetate-3-methylimidazole salt Chemical compound 0.000 claims description 5
- IAZSXUOKBPGUMV-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CCCC[NH+]1CN(C)C=C1 IAZSXUOKBPGUMV-UHFFFAOYSA-N 0.000 claims description 4
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- DETSYOQNWCXITA-UHFFFAOYSA-N C(C1=CC=CC=C1)N1CN(C=C1)C.C(C)(=O)O Chemical compound C(C1=CC=CC=C1)N1CN(C=C1)C.C(C)(=O)O DETSYOQNWCXITA-UHFFFAOYSA-N 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010061481 Renal injury Diseases 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 208000037806 kidney injury Diseases 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000017074 necrotic cell death Effects 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000019624 protein content Nutrition 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Abstract
The invention discloses a method for detecting heavy metal chromium in food, which comprises the following steps: step one, taking solid food to be detected, cleaning, crushing, freeze-drying and grinding to obtain powder; adding hydrophilic ionic liquid and acetic acid into the powder, uniformly stirring, soaking for 30-60 min at 30-40 ℃, filtering, and filtering to obtain a filtrate and a first liquid; adding the filtrate into a mixed solution of hydrochloric acid and nitric acid, uniformly stirring, then placing the mixed solution into a closed reactor, gradually heating to 120-130 ℃, preserving heat for 4-5 hours, cooling to room temperature, and filtering to obtain a second liquid; step four, mixing the first liquid and the second liquid at normal temperature to obtain liquid to be detected; and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry. The chromium content measured by the method is closer to the actual chromium content in the food.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to a method for detecting heavy metal chromium in food.
Background
Chromium is one of the essential microelements in the human body, a proper amount of chromium plays a key role in maintaining human health, but chromium is taken as a heavy metal element, and excessive chromium can cause threat to human health in the human body, for example, excessive chromium-containing compounds enter the human body to possibly cause kidney injury, cause change of kidney functions and enzyme and protein contents in urine, and seriously possibly cause kidney necrosis. People ingest chromium from daily diet, and most of foods contain chromium, such as meat, grains, bran and the like, and as people's living standard improves, importance is attached to the food safety, and understanding of the heavy metal content in the food is more and more important, so that the design of a detection method of heavy metal chromium in the food has great significance.
Disclosure of Invention
It is an object of the present invention to solve at least the above problems and to provide at least the advantages to be described later.
The invention also aims to provide a method for detecting heavy metal chromium in food, which comprises the steps of firstly soaking a sample to be detected by using hydrophilic ionic liquid and acetic acid, weakening the attaching effect of the chromium to the sample to be detected, then digesting the sample to be detected under the high-temperature and high-pressure acidic environment, so that the chromium in the sample to be detected is more thoroughly separated, and the detection value of the chromium is more close to the actual chromium content in the food.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for detecting heavy metal chromium in food, comprising the steps of:
step one, taking solid food to be detected, cleaning, crushing, freeze-drying and grinding to obtain powder;
adding acetic acid and a hydrophilic ionic liquid solution into the powder, uniformly stirring, soaking for 30-60 min at 30-40 ℃, filtering, and filtering to obtain a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid, uniformly stirring, then placing the mixed solution into a closed reactor, gradually heating to 120-130 ℃, preserving heat for 4-5 hours, cooling to room temperature, and filtering to obtain a second liquid;
step four, mixing the first liquid and the second liquid at normal temperature to obtain liquid to be detected;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
Preferably, in the method for detecting heavy metal chromium in food, the grain size of the milled powder in the first step is 0.5-2 mm.
Preferably, in the method for detecting heavy metal chromium in food, the volume ratio of acetic acid to hydrophilic ionic liquid solution in the second step is (3-5): 1.
preferably, in the method for detecting heavy metal chromium in food, the concentration of the hydrophilic ionic liquid solution is 0.8-1.6 mol/L.
Preferably, in the method for detecting heavy metal chromium in food, the hydrophilic ionic liquid is one of 1-ethyl-3-methylimidazole acetate, 1-benzyl-3-methylimidazole acetate and 1-butyl-3-methylimidazole chloride.
Preferably, in the method for detecting heavy metal chromium in food, the second step is to irradiate with infrared rays while soaking, then electrify for 30-50 s, and then filter.
Preferably, in the method for detecting heavy metal chromium in food, the volume ratio of hydrochloric acid to nitric acid in the third step is (3-5): (1-2).
Preferably, in the method for detecting heavy metal chromium in food, in the third step, the filtrate is added into a mixed solution of hydrochloric acid and nitric acid, and after being uniformly stirred, the mixture is soaked and stirred for 20-40 min at 35-50 ℃, and then the mixture is placed into a closed reactor.
Preferably, in the method for detecting heavy metal chromium in food, the temperature rising rate in the reaction process in the closed reactor in the step three is 30 ℃/min.
The invention at least comprises the following beneficial effects: in the method, the infrared irradiation is utilized to increase the activity degree of molecules, thereby accelerating the reaction speed; in the method, hydrophilic ionic liquid and acetic acid are used for acting on a sample to be tested, so that the attaching action of chromium on the sample to be tested is weakened, the chromium is more easily separated from the sample to be tested, and then the chromium is enriched by electrifying, so that the chromium in the sample to be tested is more thoroughly separated in the digestion process of the sample to be tested under the high-temperature and high-pressure acidic environment; the detection value of chromium in the food is very close to the actual chromium content in the food.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments so that those skilled in the art can practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The experimental methods described in the following embodiments are conventional methods unless otherwise indicated, and the reagents and materials are commercially available.
Example 1:
step one, taking 100g of rice to be detected with known chromium content, cleaning, crushing, freeze-drying, and grinding to powder with the particle size of 0.5mm to obtain powder;
step two, adding the powder into the powder with the volume ratio of 3:1 and 1-ethyl-3-methylimidazole acetate solution with the concentration of 0.8mol/L until the acetic acid and the solution are immersed, stirring the mixture uniformly, immersing the mixture at the temperature of 30 ℃ and simultaneously irradiating the mixture for 30min by infrared rays, then electrifying the mixture for 30s, filtering the mixture, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 5:2, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 20min at 35 ℃, then placing the mixed solution into a closed reactor, gradually heating to 120 ℃ at a heating rate of 30 ℃/min, preserving heat for 4h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 1.
Example 2
Step one, taking 100g of rice to be detected with known chromium content, cleaning, crushing, freeze-drying, grinding to powder with the particle size of 1mm to obtain powder;
step two, adding the powder into the powder with the volume ratio of 4:1 and 1-benzyl-3-methylimidazole acetate solution with the concentration of 1.2mol/L until the solution is immersed, stirring uniformly, immersing at 35 ℃ while irradiating with infrared rays for 45min, then electrifying for 40s, filtering, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 3:1, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 30min at 40 ℃, then placing the mixed solution into a closed reactor, gradually heating to 125 ℃ at a heating rate of 30 ℃/min, preserving heat for 4.5h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 1.
Example 3
Step one, taking 100g of rice to be detected with known chromium content, cleaning, crushing, freeze-drying, grinding to powder with the particle size of 2mm to obtain powder;
step two, adding the powder with the volume ratio of 5:1 and 1-butyl-3-methylimidazole chloride solution with the concentration of 1.6mol/L until the acetic acid and the solution are immersed, stirring the mixture uniformly, immersing the mixture at the temperature of 40 ℃ and simultaneously irradiating the mixture for 60 minutes by infrared rays, then electrifying the mixture for 50 seconds, filtering the mixture, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 4:1, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 40min at 50 ℃, then placing the immersed solution into a closed reactor, gradually heating to 130 ℃ at a heating rate of 30 ℃/min, preserving heat for 5h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 1.
Example 4
Step one, taking 100g of peanuts with known chromium content to be detected, cleaning, crushing, freeze-drying, grinding to powder with the particle size of 0.5mm to obtain powder;
step two, adding the powder into the powder with the volume ratio of 3:1 and 1-ethyl-3-methylimidazole acetate solution with the concentration of 0.8mol/L until the acetic acid and the solution are immersed, stirring the mixture uniformly, immersing the mixture at the temperature of 30 ℃ and simultaneously irradiating the mixture for 30min by infrared rays, then electrifying the mixture for 30s, filtering the mixture, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 5:2, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 20min at 35 ℃, then placing the mixed solution into a closed reactor, gradually heating to 120 ℃ at a heating rate of 30 ℃/min, preserving heat for 4h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 2.
Example 5
Step one, taking 100g of pig liver to be detected with known chromium content, cleaning, crushing, freeze-drying, and grinding to obtain powder with the particle size of 1 mm;
step two, adding the powder into the powder with the volume ratio of 4:1 and 1-benzyl-3-methylimidazole acetate solution with the concentration of 1.2mol/L until the solution is immersed, stirring uniformly, immersing at 35 ℃ while irradiating with infrared rays for 45min, then electrifying for 40s, filtering, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 3:1, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 30min at 40 ℃, then placing the mixed solution into a closed reactor, gradually heating to 125 ℃ at a heating rate of 30 ℃/min, preserving heat for 4.5h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 2.
Example 6
Step one, taking 100g of potatoes to be detected with known chromium content, cleaning, crushing, freeze-drying, grinding to powder with the particle size of 2mm, and obtaining powder;
step two, adding the powder with the volume ratio of 5:1 and 1-butyl-3-methylimidazole chloride solution with the concentration of 1.6mol/L until the acetic acid and the solution are immersed, stirring the mixture uniformly, immersing the mixture at the temperature of 40 ℃ and simultaneously irradiating the mixture for 60 minutes by infrared rays, then electrifying the mixture for 50 seconds, filtering the mixture, and obtaining a filtrate and a first liquid;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 4:1, uniformly stirring, immersing the filtrate in the mixed solution, soaking and stirring for 40min at 50 ℃, then placing the immersed solution into a closed reactor, gradually heating to 130 ℃ at a heating rate of 30 ℃/min, preserving heat for 5h, cooling to room temperature, and filtering to obtain a second liquid;
mixing the first liquid and the second liquid at normal temperature, and adding proper deionized water for dilution to obtain liquid to be tested;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 2.
Comparative example 1
The same as in example 2, except that: and no infrared irradiation is performed in the second step.
Comparative example 2
The same as comparative example 1, except that: the soaking time in the second step is 55min.
Comparative example 3
The same as in example 2, except that: and in the second step, no power-on process is performed.
Comparative example 4
The same as in example 2, except that: in the second step, no 1-benzyl acetate-3-methylimidazole salt solution is added.
Comparative example 5
The same as in example 2, except that: acetic acid is not added in the second step.
Comparative example 6
The same as in example 2, except that: the acetic acid and the 1-benzyl acetate-3-methylimidazole salt solution added in the second step are replaced by water.
Comparative example 7
The same as in example 2, except that: acetic acid is not added in the second step, and no electrifying process is adopted.
Comparative example 8
The same as in example 2, except that: in the second step, no 1-benzyl acetate-3-methylimidazole salt solution is added, and no electrifying process is adopted.
Comparative example 9
The same as in example 2, except that: and (3) no step II and operation related to the substances in the step II are carried out, and the solid food is directly digested by acid under the high-temperature and high-pressure condition to obtain chromium in the food.
Step one, taking 100g of rice to be detected with known chromium content, cleaning, crushing, freeze-drying, grinding to powder with the particle size of 1mm to obtain powder;
adding the powder into a mixed solution of hydrochloric acid and nitric acid in a volume ratio of 3:1, uniformly stirring, immersing the filtered material in the mixed solution, soaking and stirring for 30min at 40 ℃, then placing the mixed solution into a closed reactor, gradually heating to 115 ℃ at a heating rate of 30 ℃/min, preserving heat for 13min, cooling to room temperature, filtering, adding proper deionized water, and diluting to obtain a liquid to be detected;
and thirdly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
The test was performed three times, and the test results were averaged and recorded in table 1.
In the above embodiments: the concentration of nitric acid is 68%, the concentration of hydrochloric acid is 36%, and the concentration of acetic acid is 5%.
Comparative example 10
By usingThe rice to be detected with known chromium content is detected by the detection method in (3), the detection is carried out three times, and the average value of the detection results is calculated and recorded in the table 1.
From the analysis of the test results in Table 1, it is clear that the chromium content of the rice measured by the method of the present invention is very close to the actual chromium content; in combination with the analysis of the test results of comparative example 1, comparative example 2 and example 2, both increased irradiation of infrared rays and increased reaction time period led to more chromium precipitation, because irradiation of infrared rays in the present invention increased the reaction rate of the powder with acetic acid and the hydrophilic ionic liquid, and thus the test result of comparative example 2 was also similar to the true value, but the time taken was longer than that of the method of the present invention; in combination with the analysis of the test results of comparative examples 4, 5, 6, 7, 8, 9 and 2, the effect of enriching chromium to precipitate more thoroughly during the digestion in step three was not achieved even if the power was turned on because no acetic acid and hydrophilic ion solution acted on the powder together, but the attaching effect of chromium to the powder could not be weakened, so the test result was not different from that of comparative example 9; in comparative example 3, acetic acid and a hydrophilic ion solution act on the powder together to weaken the attaching effect of chromium on the powder and increase the possibility of chromium precipitation, so that the test result is slightly increased compared with comparative examples 4 and 5, but the chromium precipitation in the digestion process of step three is not thorough due to the lack of the chromium enrichment process in the electrifying process, and the test result is smaller than that of example 2.
From the analysis of the test results in table 2, the chromium content of the various foods as determined by the method of the present invention was very close to its actual content.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.
Claims (5)
1. The method for detecting the heavy metal chromium in the food is characterized by comprising the following steps of:
step one, taking solid food to be detected, cleaning, crushing, freeze-drying and grinding to obtain powder;
adding acetic acid and a hydrophilic ionic liquid solution into the powder, uniformly stirring, soaking at 30-40 ℃ and simultaneously irradiating with infrared rays for 30-60 min, then electrifying for 30-50 s, and filtering to obtain a filtrate and a first liquid; the volume ratio of acetic acid to hydrophilic ionic liquid solution is (3-5): 1, a step of; the concentration of the hydrophilic ionic liquid solution is 0.8-1.6 mol/L;
wherein the hydrophilic ionic liquid is one of 1-ethyl-3-methylimidazole acetate, 1-benzyl acetate-3-methylimidazole salt and 1-butyl-3-methylimidazole chloride salt;
adding the filtrate into a mixed solution of hydrochloric acid and nitric acid, uniformly stirring, then placing the mixed solution into a closed reactor, gradually heating to 120-130 ℃, preserving heat for 4-5 hours, cooling to room temperature, and filtering to obtain a second liquid;
step four, mixing the first liquid and the second liquid at normal temperature to obtain liquid to be detected;
and fifthly, detecting the chromium content in the liquid to be detected by using an atomic absorption spectrometry.
2. The method for detecting heavy metal chromium in food according to claim 1, wherein the particle size of the milled powder in the first step is 0.5-2 mm.
3. The method for detecting heavy metal chromium in food according to claim 1, wherein in the third step, the volume ratio of hydrochloric acid to nitric acid is (3-5): (1-2).
4. The method for detecting heavy metal chromium in food according to claim 1, wherein in the third step, the filtrate is added into a mixed solution of hydrochloric acid and nitric acid, and after being uniformly stirred, the mixture is soaked and stirred for 20-40 min at 35-50 ℃, and then the mixture is placed into a closed reactor.
5. The method for detecting chromium as claimed in claim 1, wherein the temperature rise rate in the reaction process in the closed reactor in the third step is 30 ℃/min.
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