CN110609004B - Analysis and detection method for chromium metal element in solid food sample - Google Patents
Analysis and detection method for chromium metal element in solid food sample Download PDFInfo
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Abstract
The invention provides a method for analyzing and detecting chromium metal elements in a solid food sample, which comprises the following steps: (1) dissolving a solid food sample by using hydrophilic ionic liquid; (2) adding deionized water to precipitate out cellulose, and filtering; (3) and (3) detecting the chromium content of the aqueous solution of the hydrophilic ionic liquid by using a graphite furnace atomic absorption spectrometry. The method has the advantages of high sensitivity, strong universality, simple and convenient operation and the like.
Description
Technical Field
The invention belongs to the field of food safety, and particularly relates to an analysis and detection method for chromium metal elements in a solid food sample.
Background
Heavy metal, as a ubiquitous environmental pollutant, can cause very big hidden danger for food safety, is the food pollutant that needs strict control, therefore it is very important to carry out detection and analysis to the heavy metal ion in the food solid sample. Chromium as a heavy metal is accumulated in a human body to a certain degree to generate irreversible harm, heavy metal elements are difficult to degrade and discharge in organisms, and heavy metals in the environment can be enriched into food required by human daily life by thousands of times through a food chain.
Chromium is used in a wide range of applications in modern industries, such as the automotive industry, where chromium is used to manufacture parts; as in the audio and video industry, chromium is used to make magnetic and video tapes. Chromium can also be used for producing stainless steel, or for material plating rust prevention, and the like. The biological toxicity of the chromium element is related to the valence state of the chromium element, trivalent chromium is beneficial to human bodies, but the trivalent chromium is not easy to be absorbed by the human bodies, and the trivalent chromium is usually discharged out of the human bodies along with metabolism after entering the human bodies. Hexavalent chromium has a very strong oxidizing property, is harmful to the human body, is easily absorbed by the human body, and is easily deposited in the human body. When people eat hexavalent chromium by mistake, symptoms such as nausea, vomiting, strong abdominal pain and the like occur, and people die when taking hexavalent chromium excessively.
If the content of chromium in the soil is too high, the chromium can also have adverse effects on the growth of crops, and related documents report that: the research shows that the hexavalent chromium in the soil is easily absorbed by plants due to the existence form of the hexavalent chromium in the soil, and the hexavalent chromium is also shown to be easier to enter a food chain and be enriched through the food chain. However, the transferability of chromium in plant plants is poor in general, most of trivalent chromium and hexavalent chromium absorbed by plants are concentrated on roots, and chromium capable of transferring to leaves and stems is only 1/77-1/1633 of chromium elements of the roots.
The chromium element taken in daily diet of people mainly comes from animal livers, and most crops also contain trace chromium. Chromium is a very critical trace element in human body, and is distributed in a plurality of parts of human body, such as skeletal muscle, brain and the like, and is related to the development of human body and blood sugar metabolism. When the human body is lack of chromium, the symptom of blood sugar metabolism disorder can be caused, or diseases such as diabetes and the like can be caused, trivalent chromium is also related to the control of cholesterol, and when the concentration of the trivalent chromium is too low, heart diseases can be caused. Trivalent chromium is considered as an element beneficial to the human body and is an essential element for sugar metabolism and lipid metabolism of the human body, but studies have also shown that excessive intake of trivalent chromium damages DNA in the human body.
Because the composition of food samples, especially solid food samples, is complex, the content of heavy metal ions is low, and part of heavy metal elements also have diversity of valence states and forms, the method for detecting and analyzing the content of heavy metal ions in food needs to be further improved at present.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent or to at least provide a useful commercial choice. Therefore, an object of the present invention is to provide a method for analyzing and detecting chromium metal elements in a solid food sample, which has the advantages of high sensitivity, strong universality, and simple operation, and overcomes the problem that the detection of graphite furnace atomic absorption spectrometry by ionic liquid has influence such as inhibition and interference.
The invention provides a method for analyzing and detecting chromium metal elements in a solid food sample. According to an embodiment of the invention, the method comprises: (1) dissolving a solid food sample by using hydrophilic ionic liquid; (2) adding deionized water to precipitate out cellulose, and filtering; (3) and (3) detecting the chromium content of the aqueous solution of the hydrophilic ionic liquid by using a graphite furnace atomic absorption spectrometry.
In the present invention, since most of the organic matter (cellulose) in the liquid phase is precipitated in advance, the liquid phase portion which is finally detected in the graphite furnace is an aqueous solution of a hydrophilic ionic liquid containing a very small amount of organic matter (organic matter such as lignin). The cellulose is prevented from directly entering a graphite furnace and is difficult to completely incinerate, and the follow-up detection is very convenient.
The term "contacting" as used herein is to be understood broadly and can be any means that enables at least two reactants to react chemically, e.g. mixing of two reactants under suitable conditions.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The method for analyzing and detecting the chromium metal element in the solid food sample according to the embodiment of the invention can also have the following additional technical characteristics:
according to the embodiment of the invention, the hydrophilic ionic liquid is an ionic liquid composed of imidazole cations, halogen element anions or acetate anions. Therefore, a pretreatment scheme of the graphite furnace atomic absorption spectrometry, which is environment-friendly, economical and efficient, can be found by utilizing the good dissolving performance and the characteristics of the hydrophilic ionic liquid for cellulose.
According to an embodiment of the present invention, the hydrophilic ionic liquid is 1, 3-dibenzylimidazole acetate, 1- (2-naphthylmethyl) -3-methylimidazole acetate, 1-heptyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate, at least one of 1-acetic acid benzyl-3-methylimidazolium salt, 1- (cyclohexylmethyl) -3-methylimidazolium acetate and 1-butyl-3-methylimidazolium chloride salt, preferably at least one of 1-ethyl-3-methylimidazolium acetate, 1-acetic acid benzyl-3-methylimidazolium salt and 1-butyl-3-methylimidazolium chloride salt, and most preferably 1-butyl-3-methylimidazolium chloride salt. Therefore, the sample to be analyzed can be rapidly dissolved under the condition of ensuring that the composition structure of the sample is unchanged, so that the subsequent analysis and detection of heavy metal ions are facilitated.
According to an embodiment of the present invention, the ratio of the amount of the solid food sample to the amount of the hydrophilic ionic liquid is (0.2 to 0.4) g: 3g of the total weight. According to the embodiment of the invention, the dosage of the deionized water is 50 mL. The concentration of [ Bmim ] -Cl in the aqueous solution at this time was 0.06 g/mL.
According to embodiments of the present invention, there is no need to add [ Bmim ] to the ionic liquid]-aqueous solution of Cl adding HNO 3 。
According to an embodiment of the present invention, the step (2) further comprises filtering with a 0.22 μm microporous membrane after adding deionized water. Therefore, the purpose of removing heavy metal ion impurities in the ionic liquid can be achieved.
According to an embodiment of the present invention, the graphite furnace atomic absorption spectrometry measures the wavelength: measuring wavelength: 357.9nm, lamp current: 7.0mA, slit 0.2nm, background subtraction mode: the background of the Zeeman buckle, the sample amount is 10 mu L, the sample amount of the matrix improving agent is 10 mu L, the data is recorded by adopting the peak height, and the temperature rising program of the graphite furnace is as follows:
according to the embodiment of the invention, the ashing temperature during the test is optimized. The preferred ashing temperature is 1300 ℃. Therefore, the interference of the ionic liquid [ Bmim ] -Cl on the measurement signal of the Cr element in different degrees can be effectively eliminated. The ashing temperature is increased to achieve more complete ashing, interference to a certain degree can be eliminated, and excessive ashing temperature can also cause loss of heavy metal elements.
According to the embodiment of the invention, ammonium dihydrogen phosphate is selected as the matrix improver. Because the ionic liquid [ Bmim ] -Cl contains imidazole cations and chloride ions, under the condition that no matrix improver is added or the ashing temperature is low, the detection of Cr element in the ionic liquid [ Bmim ] -Cl aqueous solution by using graphite furnace atomic absorption spectrometry can be interfered.
According to a specific embodiment of the present invention, the concentration of the ammonium dihydrogen phosphate solution is 2% by mass. The impact of the higher ashing temperature selected in this study can thus be avoided.
This application utilizes ionic liquid to the good solubility of solid food sample, will treat the sample of analysis and dissolve fast under guaranteeing the unchangeable condition of its constitutional structure to make things convenient for follow-up heavy metal ion's analysis and detection, this application is through the quick solution of hydrophilicity ionic liquid to solid food sample, replaces the process of clearing up of present universal adoption, from the safety and the environmental pollution problem that the preceding processing technique of the heavy metal ion detection analysis in the present solid food sample exists at the root.
According to the method for analyzing and detecting the chromium metal element in the solid food sample, at least one of the following advantages can be realized:
1. the analysis and detection method provided by the embodiment of the invention is green and environment-friendly, can achieve the purpose of pretreatment by using few chemical reagents, and has little pollution to the environment. The method is simple, convenient and quick (can be completed within about half an hour), and compared with wet digestion which requires 2-4 hours and microwave digestion which requires about 1.5-2 hours, the efficiency is greatly improved;
2. according to the analysis and detection method provided by the embodiment of the invention, the pretreatment reaction condition is mild, the consumption of a large amount of strong acid and strong oxidant reagents is avoided, harsh reaction conditions such as high temperature and high pressure are not required, the operation environment of an analyst is improved, and the health and safety of the analyst can be guaranteed;
3. according to the analytical detection method of the embodiment of the invention, 0.5mLHNO is used 3 3g of Ionic liquid [ Bmim ]]-Cl dissolved 0.3g of sample for 5min at a heating temperature of 160 ℃. The accuracy of the detection result of the heavy metal Cr content is 95.74-104.08%, the recovery rate is 95.04-103.36%, the detection limit of the Cr element is 0.145 mug/L, and when the sample weighing amount is 0.2g and the volume fixing volume is 50mL, the detection limit of the Cr element is 0.04 mg/kg.
4. The invention provides a novel, simple, convenient, rapid, green and safe pretreatment method for analyzing and detecting the heavy metal Cr in the sample. The method is essentially different from the application of the ionic liquid reported in the current literature in the aspect of heavy metal ion detection and analysis, no relevant literature report is found, and the method has original innovation.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a graph showing the influence of ashing temperature on Cr element detection signal values according to example 3 of the present invention;
FIG. 2 shows a calibration curve of a Cr solution according to example 4 of the present invention.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The specific techniques or conditions not indicated in the examples are performed according to the techniques or conditions described in the literature in the field or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The dried mushroom, the dried agaric and the dried tea solid samples are purchased from the market, stirred for 15min by using a stirrer, screened by a 100-mesh screen, then dried for 5h in a constant-temperature oven with the temperature set to be 100 ℃, and stored in a dry place for later use.
The main reagents are as follows: concentrated nitric acid (analytically pure, 68% strength), perchloric acid (analytically pure, 70% strength), hydrochloric acid (analytically pure, 36.5% strength), a multi-element mixed standard solution (GBW08607), ammonium dihydrogen phosphate (analytically pure), and ammonium dihydrogen phosphate solution (2% strength).
Mixing standard solutions: the mixed standard solution of Pb, Cr, Cd and other elements purchased from China institute of metrology science, wherein the concentration of Pb is 1.03 mu g/g, the concentration of Cd is 0.104 mu g/g, and the concentration of Cr is 0.516 mu g/g.
Ionic liquid (1-butyl-3-methylimidazolium chloride, [ Bmim ] -C1): CAS: 79917-90-1, obtained from commercial sources, with a concentration of 99.9%.
Main experimental apparatus and equipment: an atomic absorption spectrophotometer (AA280Z), a chromium hollow cathode lamp, a cadmium hollow cathode lamp, a 1.5mL sample cup, a pyrolytic graphite tube, all produced by Agilent, USA; electronic balance (mettleltolo-tomado limited), muffle FO610C (yamata japan), vacuum oven (memott trade limited).
EXAMPLE 1 preparation of solutions
Mixing standard stock solutions: 2mL of the multielement mixed standard solution (GBW 08607: where the Cr concentration is 0.516. mu.g/g) was removed. Dissolving in 25mL of deionized water, shaking and shaking uniformly to obtain a mixed standard stock solution with the Cr concentration of 41.28 mu g/L.
Example 2 sample pretreatment with ionic liquid and nitric acid
Accurately weighing 3g of ionic liquid [ Bmim ]]-Cl was placed in a beaker and the beaker was heated to 90 ℃ to bring the ionic liquid [ Bmim [ ]]Melting the-Cl crystal, taking down and cooling after the Cl crystal is completely melted, accurately weighing 0.2g of sample powder into a beaker, uniformly dispersing the sample in the liquid surface, and adding 0.5mL of concentrated HNO 3 Heating to 160 ℃, dissolving for 5min, adding deionized water to precipitate cellulose, diluting to 50mL of constant volume, taking part of supernatant after the precipitated cellulose naturally settles, and detecting the supernatant by using graphite furnace atomic absorption spectrometry.
EXAMPLE 3 selection of ashing temperature
Since the aqueous solution of the ionic liquid [ Bmim ] -Cl contains organic substances, it is difficult to completely incinerate the organic substances when a low ashing temperature is used, and detection is disturbed. When the ashing temperature is within the range of 1000-1400 ℃, the light absorption value of Cr element is shown in figure 1. From the figure, it can be seen that, when the ashing temperature is lower than 1300 ℃, the detection signal is inhibited and influenced by the ionic liquid [ Bmim ] -Cl, and when the ashing temperature reaches 1300 ℃, the detection signal reaches the maximum value, and it can be seen that the optimal ashing temperature is 1300 ℃.
Example 4 Standard Curve was prepared
Transferring a proper amount of mixed standard stock solution (GBW 08607: wherein the Pb concentration is 1.03 mug/g, the Cd concentration is 0.104 mug/g and the Cr concentration is 0.516 mug/g) into a volumetric flask, and fixing the volume to the scale to prepare a series of mixed standard solutions. The series of mixed standard solutions were used, initial graphite furnace temperature program conditions were set with reference to the current national standards, and the results of instrumental automatic standard curve measurements were found in table 1.
TABLE 6 absorbance of Cr standard solutions of different concentrations
A standard curve of Cr element is shown in FIG. 2 and is shown in Table 1. Therefore, the following steps are carried out: the standard curve of the Cr solution was abs (Cr) ═ 0.0035 × C (μ g/L) +0.0452, and the correlation was 0.999. Therefore, the instrument has the characteristics of high sensitivity and good correlation.
Example 5 detection Limit determination
Due to HNO 3 And an ionic liquid [ Bmim ]]since-Cl all have an influence on the detection, the method detection limit in this embodiment needs to be obtained by performing blank experiments under the conditions of example 2, making 20 blanks for detection, performing minimum concentration labeling detection after the detection limit is obtained by the MDL calculation method, and examining the relative standard deviation, correlation coefficient, and the like. The relative standard deviation (RSD%) of blank values, and the detection limit results are shown in Table 2 (detection limit concentration is solution concentration).
TABLE 2 detection of Cr by ion liquid [ Bmim ] -Cl-graphite furnace atomic absorption spectrometry
From table 2, it can be seen that the method has a lower detection limit, and good sensitivity.
Example 6 accuracy determination
The solid samples of the three foods of dry agaric, dry mushroom and dry tea are pretreated by adopting the conditions of the embodiment 2, Cr element in the samples is analyzed, and the detection result and the accuracy result thereof are shown in a table 3.
TABLE 3 test results and accuracy results
As can be seen from Table 3, the results of detection consistent with conventional wet digestion sample detection (see GB 5009.123) can be obtained by dissolving a food solid sample using an ionic liquid [ Bmim ] -Cl as a solvent, adding 0.5mL of concentrated HNO3, and performing Cr elemental analysis using graphite furnace atomic absorption spectrometry.
Example 9 recovery determination
In this example, the heavy metal content of the sample was recovered by adding the standard 0.5 times, 1 time, and 2 times, and the number of times of the repeated measurement was 6. The recovery results of Cr elements from the samples of dried Auricularia, Lentinus Edodes and folium Camelliae sinensis are shown in Table 5.
TABLE 5 recovery of Cr from Auricularia, Lentinus Edodes, and folium Camelliae sinensis
As can be seen from Table 5, the standard recovery rates of the heavy metal content of 0.5-fold, 1-fold and 2-fold samples, which are repeatedly measured six times in each group, and the RSD of the measured values are 95.04% -103.36% and 4.11% -6.51% respectively, which indicates that the method has good sensitivity and accuracy and can meet the requirements of conventional detection.
In the description of the present invention, it is to be understood that the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the various embodiments or examples and features of the various embodiments or examples described in this specification can be combined and combined by those skilled in the art without being mutually inconsistent.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (1)
1. A method for analyzing and detecting chromium metal elements in a solid food sample is characterized by comprising the following steps:
accurately weighing 3g of 1-butyl-3-methylimidazolium chloride, placing the 1-butyl-3-methylimidazolium chloride in a beaker, heating the beaker to 90 ℃ to melt 1-butyl-3-methylimidazolium chloride crystals, taking down and cooling the beaker after the crystals are completely melted into hydrophilic ionic liquid, accurately weighing 0.2g of solid food sample powder in the beaker, uniformly dispersing the solid food sample on the liquid surface, adding 0.5mL of concentrated HNO 3 Heating to 160 ℃, dissolving for 5min, adding deionized water to precipitate cellulose, fixing the volume to 50mL, taking part of supernatant after the precipitated cellulose naturally settles, and detecting the supernatant by using a graphite furnace atomic absorption spectrometry;
optimizing the ashing temperature in the test process of the graphite furnace atomic absorption spectrometry, wherein the ashing temperature is 1300 ℃;
ammonium dihydrogen phosphate is used as a matrix improver;
the concentration of the ammonium dihydrogen phosphate solution is 2 percent by mass.
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