CN112729991A - Environment-friendly pretreatment method for determining cadmium in grain processed product based on super microwave - Google Patents
Environment-friendly pretreatment method for determining cadmium in grain processed product based on super microwave Download PDFInfo
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Abstract
The invention discloses a green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave, which comprises the following steps: the method comprises the following steps: step 1, taking a grain sample; step 2, adding hydrogen peroxide solution into the sample, uniformly mixing, and putting into a super microwave chemical platform; step 3, introducing nitrogen into the super microwave chemical platform, and keeping the pressure; step 4, carrying out digestion treatment according to a preset temperature-rising program; step 5, after the super microwave chemical platform temperature rise program is completed and cooled, taking out a sample; step 6, ultrasonic degassing; and 7, transferring the sample in the microwave digestion tank into a volumetric flask, metering the volume to a scale by using nitric acid, uniformly mixing, and finishing pretreatment. Has the advantages that: green and environment-friendly, low reagent cost, low introduced reagent blank, simple and convenient operation and high working efficiency.
Description
Technical Field
The invention relates to the field of food detection, in particular to a green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave.
Background
The processed grain product includes rice, wheat flour, dried noodles, processed grain product, milled grain product, etc. The pretreatment methods for cadmium determination according to the current national standard GB5009.15-2014 & lt & gt determination of cadmium in food safety national standard food & gt and GB 5009.268-2016 & lt & gt determination of multiple elements in food safety national standard food & gt include four pretreatment methods, namely pressure tank digestion, wet digestion, microwave digestion and dry digestion, wherein the former three pretreatment methods all use strong acid, such as nitric acid, perchloric acid and the like. The strong nitric acid can generate nitrogen monoxide, nitrogen dioxide, nitrous oxide, dinitrogen tetroxide and dinitrogen pentoxide waste gas when decomposed at high temperature and high pressure, thereby not only polluting the environment but also causing damage to operators. And the introduced reagent is blank, and perchloric acid can introduce chloride ions, so that matrix interference is caused, and the determination result is influenced. And the dry ashing may cause the volatilization loss of the low-temperature element cadmium.
Disclosure of Invention
The invention aims to provide a reagent which is green and environment-friendly, has low reagent cost, low introduced reagent blank, simple and convenient operation and high working efficiency; each sample only needs a small amount of hydrogen peroxide, so that the reagent cost is saved by 70%; strong acid is not used, and acid removing links are not needed, so that the working time is greatly reduced; the generation of nitrogen monoxide, nitrogen dioxide, nitrous oxide, dinitrogen trioxide, dinitrogen tetroxide and dinitrogen pentoxide waste gas is avoided, the loss of low-temperature element cadmium is reduced, and the determination result is accurate; and the toxic and harmful chemical reagent strong acid is not used, so that the health hazard to operators and the pollution to the environment are avoided.
The invention is realized by the following technical scheme:
the invention relates to a green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave, which comprises the following steps: the method comprises the following steps:
step 1, taking a grain processed product sample;
step 2, adding hydrogen peroxide solution into the sample, uniformly mixing, and putting into a super microwave chemical platform;
step 3, introducing nitrogen into the super microwave chemical platform, and keeping the pressure;
step 4, carrying out digestion treatment according to a preset temperature-rising program;
step 5, after the super microwave chemical platform temperature rise program is completed and cooled, taking out a sample;
step 6, carrying out ultrasonic degassing treatment on the sample in the microwave digestion tank;
and 7, transferring the sample into a volumetric flask, fixing the volume to a scale by using a nitric acid solution with the concentration of 1%, uniformly mixing, and finishing the pretreatment.
Preferably, the super microwave chemical platform comprises a magnetron, a microwave conduction device, a reaction cavity, a digestion tank and a digestion pipe; the digestion tube can be placed inside the digestion tank; one end of the microwave conduction device is connected with the bottom of the reaction cavity, and the other end of the microwave conduction device is connected with the magnetron.
Preferably, the step 1 of taking the grain processed product sample is to weigh 0.2-0.5g of the grain processed product sample into the digestion tube.
Preferably, the step 2 includes the steps of:
step a, adding 1-5mL of hydrogen peroxide solution into a digestion tube;
b, after uniformly mixing, covering a cover of the digestion tube, and placing the digestion tube in a digestion tank;
and c, placing the digestion tank in a reaction cavity of the super microwave chemical platform.
Preferably, in the step 3, nitrogen is introduced into the reaction chamber, so that the pressure in the reaction chamber is increased to 3500kPa-4500 kPa.
Preferably, the temperature raising procedure in step 4 is performed in three stages:
stage 1: heating for 5min to 130 deg.C and obtain pressure of 13000 kPa;
and (2) stage: maintaining the temperature and pressure of stage 1 for 5 min;
and (3) stage: heating for 8min to 185 deg.C and obtain an inner cavity pressure of 13000 kPa;
and (4) stage: maintaining the temperature and pressure of stage 2 for 5 min;
and (5) stage: heating for 10min to 220 deg.C, and keeping the pressure in the inner cavity at 15000 kPa;
and 6: the temperature and pressure of stage 5 were maintained for 15 min.
Preferably, the ultrasonic degassing treatment is ultrasonic degassing of the sample for 5-10min by using an ultrasonic water bath box.
Preferably, the grain processed product sample comprises rice, wheat flour, dried noodles, grain processed product, and grain milled product.
Preferably, the hydrogen peroxide solution is GR-grade hydrogen peroxide.
Preferably, the purity of the nitrogen is greater than 99.999%.
The invention has the beneficial effects that: the method is green and environment-friendly, the reagent cost is low, the introduced reagent blank is low, the operation is simple and convenient, and the working efficiency is high; each sample only needs a small amount of hydrogen peroxide, so that the reagent cost is saved by 70%; strong acid is not used, and acid removing links are not needed, so that the working time is greatly reduced; the generation of nitrogen monoxide, nitrogen dioxide, nitrous oxide, dinitrogen trioxide, dinitrogen tetroxide and dinitrogen pentoxide waste gas is avoided, the loss of low-temperature element cadmium is reduced, and the determination result is accurate; and the strong acid avoids toxic and harmful chemical reagents, thus avoiding health hazard to operators and pollution to the environment.
Detailed Description
The invention will be further illustrated with reference to specific embodiments:
example (b): a green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave comprises the following steps: the method comprises the following steps: step 1, taking a grain processed product sample, and weighing 0.3g of the grain processed product sample in a digestion tube; the grain processed product sample is rice, wheat flour, fine dried noodles, grain processed product, and grain milled product;
step 2, adding a 4 mLGR-grade hydrogen peroxide solution into the sample, uniformly mixing, covering a cover of the digestion tube, and placing the digestion tube into a digestion tank; placing the digestion tank in a reaction cavity of a super microwave chemical platform;
step 3, introducing nitrogen into the reaction cavity of the super microwave chemical platform, and maintaining the pressure to increase the pressure in the reaction cavity to 4000kPa
Step 4, carrying out digestion treatment according to a preset temperature-rising program; the preset temperature-raising program comprises six stages:
stage 1: heating for 5min to 130 deg.C and obtain pressure of 13000 kPa;
and (2) stage: maintaining the temperature and pressure of stage 1 for 5 min;
and (3) stage: heating for 8min to 185 deg.C and obtain an inner cavity pressure of 13000 kPa;
and (4) stage: maintaining the temperature and pressure of stage 2 for 5 min;
and (5) stage: heating for 10min to 220 deg.C, and keeping the pressure in the inner cavity at 15000 kPa;
and 6: the temperature and pressure of stage 5 were maintained for 15 min.
Step 5, after the super microwave chemical platform temperature rise program is completed and cooled, taking out a sample;
step 6, carrying out ultrasonic degassing treatment on the sample in the microwave digestion tank, and ultrasonically degassing the sample for 10min by using an ultrasonic water bath box;
and 7, transferring the sample in the microwave digestion tank into a volumetric flask, fixing the volume to a scale by using a nitric acid solution with the concentration of 1%, uniformly mixing, and finishing pretreatment.
The super microwave chemical platform comprises a magnetron, a microwave conduction device, a reaction cavity, a digestion tank and a digestion pipe; the digestion tube can be placed inside the digestion tank; one end of the microwave conduction device is connected with the bottom of the reaction cavity, and the other end of the microwave conduction device is connected with the magnetron.
Wherein: in step 7, the nitric acid solution used has a low concentration, does not participate in the heating process, does not generate nitrogen oxides, and can stabilize elements so that the elements are not adsorbed on the container and are consistent with the standard series of substrates.
The applicant adopts the method of the invention to carry out sample pretreatment experiments, and then adopts two methods of graphite furnace Atomic Absorption Spectrometry (AAS) and inductively coupled plasma mass spectrometry (ICP-MS) to carry out methodological verification. And the methodological verification is carried out by respectively carrying out related items such as linear correlation, reagent blank, detection limit, accuracy, precision, standard addition recovery rate and the like. Verification was performed using a physical standard sample (a standard substance certified by the country and granted a certificate for the standard substance) and a positive sample from this laboratory. The environment-friendly and green pretreatment method provided by the invention is proved to be accurate and reliable.
Firstly, the experimental data of the experimental determination results of the graphite furnace atomic absorption method are as follows:
1. and (5) performing linear correlation experiments. Y0.06165 · X +0.00283 r 0.999 ═ 0.999
TABLE 1 results of Linear correlation experiments
GB/T27404- "laboratory quality control Specification food physicochemical inspection" appendix F in the technical requirements of the inspection method determination in F.2 calibration curve, "validation method, linear correlation coefficient should not be less than 0.99. The pretreatment of the sample by adopting the pretreatment method of the invention is carried out, and then the linear correlation coefficient is 0.999 which is higher than 0.99 required by the national standard GB/T27404-.
2. Results of precision experiments
TABLE 2 results of the precision test
Calculating the formula:
the method comprises the steps of pretreating a sample according to a pretreatment method of the invention aiming at a standard sample purchased by an applicant and having a national standard substance certificate, detecting the standard sample by using a graphite furnace atomic absorption spectrometry, and repeatedly measuring 8 times, wherein the average value of the measurement is 0.406mg/kg, the SD is 0.007%, the precision RSD% of the 8 times of measurement is 1.81%, and the deviation range is 11-15% when the content of the component to be detected is 100 mu g-1mg/kg in the F.3 precision in the technical requirements confirmed by the detection method in annex F of 27404 and 2008 laboratory quality control Specification food physicochemical detection.
3. Experiment of accuracy
TABLE 3 accuracy test results
Calculating the formula:
the F.5 accuracy in the technical requirements confirmed by the detection method in appendix F of GB/T27404-2008 laboratory quality control Specification food physicochemical inspection specifies that when the true value content is between 0.010 and 10mg/kg, the deviation guide range of the measured value from the true value is-20 to + 10%. The pretreatment method is adopted for sample pretreatment, and then atomic absorption graphite furnace spectrometry is adopted for determination, so that the true value deviation of the determination result and the real standard sample is-1.5%, which is far lower than-20% - + 10% required by the national standard GB/T27404-.
4. Recovery rate experiment
Experimental results of recovery
The laboratory performed standard recovery experiments with three positive samples, rice (DM), buckwheat (QM), and rice flour (NXSC-009). The recovery rate meets the technical requirements confirmed by the detection method in appendix F of GB/T27404-2008 laboratory quality control Standard food physicochemical detection.
5. The reagent blank response values were measured 21 times consecutively on reagent blank solutions:
TABLE 522 blank test results for reagents
6. Detection limit, quantification limit.
The blank solution was measured 22 times in succession and its standard deviation was calculated 0.0202.
The detection limit of the apparatus (IDL) was 3 × SD 0.0606 ng/mL.
The limit of the method is that (LOQ) is 0.005 multiplied by 3 and 0.015mg/kg
7. Comparison between laboratories
The results of the positive samples measured by the pretreatment method of the invention and the results of the national standard measurement method adopted by other third-party detection institutions are shown in the following table. And (4) carrying out comparison and verification experiments among laboratories. The method of the invention has no obvious difference with the national standard method. The pretreatment method disclosed by the invention has good extraction efficiency on heavy metal cadmium in the sample.
TABLE 6 Positive rice sample (DM) laboratory-to-laboratory comparison test results
7. Comparison result of object standard samples among different laboratories
Table 7 laboratory comparison verification results
Secondly, the experimental data of the experimental determination result of the inductively coupled plasma mass spectrometry are as follows:
1. and (5) performing linear correlation experiments. Y0.0028. X + 3.631. 10-6 r 0.9999
TABLE 1 results of Linear correlation experiments
GB/T27404- "laboratory quality control Specification food physicochemical inspection" appendix F in the technical requirements of the inspection method determination in F.2 calibration curve, "validation method, linear correlation coefficient should not be less than 0.99. After the sample is treated by the pretreatment method, the linear correlation coefficient measured by inductively coupled plasma mass spectrometry (ICP-MS) is 0.9999, which is higher than 0.99 required by the national standard GB/T27404-.
2. Results of precision experiments
TABLE 2 results of the precision test
The formula:
the applicant selects standard samples purchased with national standard substance certificates, performs pretreatment of the samples according to the method of the invention, and then performs detection by inductively coupled plasma mass spectrometry (ICP-MS). The standard sample is subjected to 6 repeated measurements, the average value of the measurement is 0.422mg/kg, the SD is 0.009%, and the precision RSD% of the 6 measurements is far lower than the F.3 precision in the technical requirement confirmed by the detection method in appendix F of GB/T27404- "laboratory quality control Standard food Conditioning testing", wherein the required content of the component to be measured is in the range of 11-15% when 100 mug-1 mg/kg.
3. Experiment of accuracy
TABLE 3 accuracy test results
In the F.5 accuracy in the technical requirements confirmed by the detection method in appendix F of GB/T27404-2008 laboratory quality control Specification food physicochemical inspection, when the true value content is between 0.010-10mg/kg, the deviation guide range of the measured value and the true value is-20% -10%. After the pretreatment method is adopted for treatment, the detection is carried out by adopting an inductively coupled plasma mass spectrometry (ICP-MS), and the deviation of the detection is-0.5 percent and is far lower than-20 percent to +10 percent required by the national standard GB/T27404-.
4. Recovery rate experiment
Experimental results of recovery
The laboratory performed standard recovery experiments with three positive samples, rice (DM), buckwheat (QM), and rice flour (NXSC-009). The recovery rate meets the technical requirements confirmed by the detection method in appendix F of GB/T27404-2008 laboratory quality control Standard food physicochemical detection.
5. The reagent blank response values were measured 21 times consecutively on reagent blank solutions:
table 521 reagent blank measurements
6. Detection limit
The blank solution was measured 21 times in succession and its standard deviation was calculated to be 0.0013.
The detection limit of the apparatus (IDL) was 3 × SD 0.004 ng/mL.
The limit of the method is that (LOQ) is 0.0003 multiplied by 3 is 0.0009mg/kg
7. The results of the positive samples measured by the pretreatment method of the present invention and the results of the measurement methods of other third-party detection institutions in accordance with the national standards are shown in the following table. And (4) carrying out comparison and verification experiments among laboratories.
The method of the invention has no obvious difference with the national standard method. The pretreatment method disclosed by the invention has good extraction efficiency on heavy metal cadmium in the sample.
TABLE 6 Positive rice (DM) sample comparison between laboratories test results
8. Comparison result of object standard samples among different laboratories
Table 7 laboratory comparison verification results
Thirdly, comparing results of different hydrogen peroxide dosages and ultrasonic and non-ultrasonic
From this result, it was found that digestion was carried out using 4ml of hydrogen peroxide solution, and the digestion effect was the best when the ultrasonic degassing treatment was carried out.
In conclusion, the green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave has high cadmium extraction efficiency, meets all specified indexes, and is completely suitable for determining the content of heavy metal cadmium in grains and processed products thereof.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalent substitutions and modifications may be made to some features of the embodiments described above, and any modifications, equivalents, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave is characterized by comprising the following steps: the method comprises the following steps:
step 1, taking a grain processed product sample;
step 2, adding hydrogen peroxide solution into the sample, uniformly mixing, and putting into a super microwave chemical platform;
step 3, introducing nitrogen into the super microwave chemical platform, and keeping the pressure;
step 4, carrying out digestion treatment according to a preset temperature-rising program;
step 5, after the super microwave chemical platform temperature rise program is completed and cooled, taking out a sample;
step 6, carrying out ultrasonic degassing treatment on the sample in the microwave digestion tank;
and 7, transferring the sample into a volumetric flask, fixing the volume to a scale by using a nitric acid solution with the concentration of 1%, uniformly mixing, and finishing pretreatment.
2. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 1, characterized in that: the super microwave chemical platform comprises a magnetron, a microwave conduction device, a reaction cavity, a digestion tank and a digestion pipe; the digestion tube may be placed inside a digestion tank; one end of the microwave conduction device is connected with the bottom of the reaction cavity, and the other end of the microwave conduction device is connected with the magnetron.
3. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 2, characterized in that: the grain sample taking in the step 1 is to weigh 0.2-0.5g of grain processed product sample into a digestion tube.
4. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 2, characterized in that: the step 2 comprises the following steps:
step a, adding 1-5mL of hydrogen peroxide solution into a digestion tube;
b, after uniformly mixing, covering a cover of the digestion tube, and placing the digestion tube in a digestion tank;
and c, placing the digestion tank in a reaction cavity of the super microwave chemical platform.
5. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 2, characterized in that: and in the step 3, nitrogen is introduced into the reaction cavity, so that the pressure in the reaction cavity is increased to 3500kPa-4500 kPa.
6. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 2, characterized in that: the temperature raising procedure in the step 4 comprises the following six stages:
stage 1: heating for 5min to 130 deg.C and obtain pressure of 13000 kPa;
and (2) stage: maintaining the temperature and pressure of stage 1 for 5 min;
and (3) stage: heating for 8min to 185 deg.C and obtain an inner cavity pressure of 13000 kPa;
and (4) stage: maintaining the temperature and pressure of stage 2 for 5 min;
and (5) stage: heating for 10min to 220 deg.C, and keeping the pressure in the inner cavity at 15000 kPa;
and 6: the temperature and pressure of stage 5 were maintained for 15 min.
7. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 2, characterized in that: and 6, ultrasonic degassing treatment is to use an ultrasonic water bath box to carry out ultrasonic degassing on the sample for 5-10 min.
8. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 3, characterized in that: the grain processed product sample comprises rice, wheat flour, dried noodles, grain processed product, and grain milled product.
9. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 4, characterized in that: the hydrogen peroxide solution is GR-grade hydrogen peroxide.
10. The green and environment-friendly pretreatment method for determining cadmium in grain processed products based on super microwave as claimed in claim 5, characterized in that: the purity of the nitrogen is more than 99.999%.
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