CN113203812A - Detection method for determining acrylamide in soil - Google Patents
Detection method for determining acrylamide in soil Download PDFInfo
- Publication number
- CN113203812A CN113203812A CN202110493403.4A CN202110493403A CN113203812A CN 113203812 A CN113203812 A CN 113203812A CN 202110493403 A CN202110493403 A CN 202110493403A CN 113203812 A CN113203812 A CN 113203812A
- Authority
- CN
- China
- Prior art keywords
- acrylamide
- water
- sample
- soil
- standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000001514 detection method Methods 0.000 title claims abstract description 62
- 239000002689 soil Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 19
- 239000012498 ultrapure water Substances 0.000 claims abstract description 19
- 239000004927 clay Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000004743 Polypropylene Substances 0.000 claims abstract description 4
- -1 polypropylene Polymers 0.000 claims abstract description 4
- 229920001155 polypropylene Polymers 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 24
- 238000004811 liquid chromatography Methods 0.000 claims description 17
- 239000012086 standard solution Substances 0.000 claims description 11
- 238000007865 diluting Methods 0.000 claims description 9
- 238000002137 ultrasound extraction Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000002474 experimental method Methods 0.000 claims description 7
- 238000002372 labelling Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000013375 chromatographic separation Methods 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 3
- 239000011043 treated quartz Substances 0.000 claims description 3
- 239000012224 working solution Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000006228 supernatant Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 abstract 4
- 239000012496 blank sample Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 24
- 238000004458 analytical method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 229920002401 polyacrylamide Polymers 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 238000011088 calibration curve Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000003516 soil conditioner Substances 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 208000012661 Dyskinesia Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Quality & Reliability (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a detection method for detecting acrylamide in soil, which comprises the following steps: s1, sample pretreatment: placing a soil sample in a polypropylene centrifugal tube with a cover, ultrasonically extracting with ultrapure water, centrifuging, taking supernatant, and filtering to be tested; s2, detecting acrylamide in the soil under the optimal liquid chromatograph condition to obtain a linear equation, a correlation coefficient and a detection limit of the acrylamide: s3, under the experimental condition of the step S2, the precision and accuracy of the marked blank sample and the powder clay sample are tested. In the invention, the detection limit of acrylamide in soil determined by the method is 0.02mg/kg, the standard recovery rate of a soil sample is 77.1-99.5%, and the relative standard deviation is 3.3-9.4%.
Description
Technical Field
The invention relates to the technical field of detection of acrylamide in soil, in particular to a detection method for detecting acrylamide in soil.
Background
Acrylamide is a water-soluble micromolecular organic matter used in the industries of papermaking, wood and textile, and the polymer polyacrylamide is widely applied at home and abroad as an artificially synthesized soil conditioner. Polyacrylamide is nontoxic, but can be degraded in soil to generate a toxic substance, namely acrylamide, which is classified as a possible human class 2 carcinogen (IIA) by the International research center for cancer (IARC) and is metabolized and converted into methacrylamide in a human body. Acrylamide in soil can be absorbed by human body directly or via underground water through skin and oral cavity, thereby causing neurointoxication and abnormal movement.
In the prior art, the food industry has more researches on the determination of acrylamide, and more methods for determining acrylamide in water by utilizing LC-MS, HPLC and GC in the aspect of environment are provided, but the research on the determination of the acrylamide content in soil is only reported. Although the current research cannot prove that the polyacrylamide as a soil conditioner has negative effects on the environment, whether the polyacrylamide generates pollution or not is still a problem worthy of attention and intensive research along with the increasing application amount, the change of factors such as the soil environment and the like. Therefore, there is a lack of a detection method for measuring acrylamide in soil.
Disclosure of Invention
In order to solve the problems and defects mentioned in the background art, a detection method for detecting acrylamide in soil is provided.
In order to achieve the purpose, the invention adopts the following technical scheme:
a detection method for detecting acrylamide in soil comprises the following steps:
s1, sample pretreatment: accurately weighing 10.00g of soil sample in a 50mL polypropylene centrifuge tube with a cover, performing ultrasonic extraction for 30min by using 20mL ultrapure water, centrifuging for 3min at 8000r/min, and filtering supernate by using a 0.45-micrometer water system needle filter to be detected.
S2, detecting acrylamide in soil under the optimal liquid chromatograph conditions:
the chromatographic conditions are as follows: a chromatographic column: ZORBAX Eclipse Plus C18 column (4.6X 100mm, 3.5 μm); mobile phase methanol: water (volume ratio 5: 95) with flow rate of 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 μ L.
S3, carrying out chromatographic separation experiments by a controlled variable method under the conditions of different mobile phase proportions, flow rate change and detection wavelength to verify the optimal liquid chromatographic conditions, wherein the liquid chromatographic conditions under the controlled variable method can adopt the following three methods:
the first method comprises the following steps: fixing other liquid chromatography conditions unchanged: the flow rate is 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; changing the mobile phase: methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90);
and the second method comprises the following steps: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; the flow rate was varied: 0.3-0.6 mL/min;
and the third is that: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the flow rate is 0.5 mL/min; the column temperature is 30 ℃; sample introduction amount: 5 mu L of the solution; changing the detection wavelength: 190-400 nm;
s4, obtaining the linear equation, correlation coefficient and detection limit of acrylamide under the experiment of step S2:
s41, accurately weighing an acrylamide standard substance with the purity of 99.9 percent into a 50mL volumetric flask, dissolving, diluting and fixing the volume by using ultrapure water, and preparing an acrylamide standard solution with the concentration of 1000 mu g/mL; then taking a proper amount of acrylamide standard solution, diluting with ultrapure water, fixing the volume, and preparing into 100 mu g/mL acrylamide standard use solution;
s42, respectively taking 100 mu g/mL acrylamide standard use solution into blank ultrapure water, diluting step by step to prepare serial standard working solutions with mass concentrations of 0.05 mu g/mL, 0.10 mu g/mL, 0.50 mu g/mL, 1.00 mu g/mL and 5.00 mu g/mL;
s43, analyzing the mixture sequentially from low concentration to high concentration by a liquid chromatograph, determining the qualitative retention time and the quantitative peak area to obtain a linear equation and a correlation coefficient of the mixture;
s44, calculation of acrylamide detection limit: adding 40 mu L of acrylamide standard solution with the concentration of 10 mu g/mL into 10g of treated quartz sand (replacing a blank soil sample), performing ultrasonic extraction for 30min by using 20mL of ultrapure water, centrifuging, taking supernate to be tested, repeatedly measuring for 7 times according to a test method, calculating the standard deviation S of the measured value, and calculating the detection limit of the soil sample by using 3 times of standard deviation:
wherein, the calculation formula of the detection limit is as follows: MDL ═ t(n-1,0.99)*S，
Wherein, MDL-method detection limit;
t-degree of freedom is (n-1), and t distribution with a confidence of 99% is (n-7, t-3.143);
s-standard deviation of n replicates;
n-the number of replicates of the sample;
s5, under the experimental conditions of the step S2, the carclazyte soil sample is subjected to labeling: after acrylamide is added into the blank soil sample, measuring for 6 times according to the whole sequence of the step S2, and measuring the precision and the accuracy of the blank soil sample after the standard addition;
s6, labeling the treated mealy clay under the experimental conditions of step S2: and (4) after the powdery clay sample is taken and added with acrylamide, measuring for 6 times according to the whole procedure of the step S2, and measuring the precision and the accuracy of the powdery clay sample after the standard addition.
As a further description of the above technical solution:
in step S3, the first flow ratio under the controlled variable method is methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90).
As a further description of the above technical solution:
in step S3, the second flow rates in the controlled variable method are 0.3mL/min, 0.4mL/min, 0.5mL/min, and 0.6mL/min, respectively.
As a further description of the above technical solution:
in step S3, the detection wavelengths of the third kind in the controlled variable method are 190nm, 200nm, and 210nm, respectively.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. in the invention, the content of acrylamide in soil is determined by establishing a high performance liquid chromatography through determining the conditions of a liquid chromatograph, and the result shows that: the method has the advantages of rapidness, accuracy, short pretreatment time, low detection limit and the like, the extractant and the mobile phase are basically ultrapure water, the environmental pollution is less, the accuracy and the precision are better, and the method is suitable for detection and analysis of the acrylamide in the soil.
2. In the present invention, the results of the liquid chromatography of acrylamide by the controlled variable method were used to verify that "mobile phase methanol: water (volume ratio 5: 95) with flow rate of 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mul' is the best liquid chromatogram condition for detecting acrylamide in soil.
Drawings
FIG. 1 is a schematic diagram illustrating a calibration curve of acrylamide in a soil according to an exemplary detection method of the present invention;
FIG. 2 is a schematic liquid chromatogram showing the concentration of 1.0 μ g/mL acrylamide in the detection method for detecting acrylamide in soil according to the embodiment of the invention;
FIG. 3 is a schematic diagram of a liquid chromatogram after adding 2.40 μ g acrylamide to silty clay under a detection method for detecting acrylamide in soil according to an embodiment of the present invention;
FIG. 4 is a schematic diagram showing a spectral scan of acrylamide at a detection wavelength of 190-400nm under a detection method for detecting acrylamide in soil according to an embodiment of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1-3, a method for detecting acrylamide in soil includes the following steps:
s1, sample pretreatment: accurately weighing 10.00g of soil sample in a 50mL polypropylene centrifuge tube with a cover, performing ultrasonic extraction for 30min by using 20mL ultrapure water, centrifuging for 3min at 8000r/min, and filtering supernate by using a 0.45-micrometer water system needle filter to be detected.
The acrylamide is a compound which is strong in polarity and very easy to dissolve in water, so that ultrapure water is selected as an extraction solvent, the acrylamide in a soil sample can be completely dissolved in water through ultrasonic extraction, then the solution is centrifuged at a high speed, and the supernatant is filtered and is to be detected.
S2, detecting acrylamide in soil under the optimal liquid chromatograph conditions:
the chromatographic conditions are as follows: a chromatographic column: ZORBAX Eclipse Plus C18 column (4.6X 100mm, 3.5 μm); mobile phase methanol: water (volume ratio 5: 95) with flow rate of 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 μ L.
S3, carrying out chromatographic separation experiments by a controlled variable method under the conditions of different mobile phase proportions, flow rate change and detection wavelength to verify the optimal liquid chromatographic conditions, wherein the liquid chromatographic conditions under the controlled variable method can adopt the following three methods:
the first method comprises the following steps: fixing other liquid chromatography conditions unchanged: the flow rate is 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; changing the mobile phase: methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90);
and the second method comprises the following steps: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; the flow rate was varied: 0.3-0.6 mL/min;
and the third is that: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the flow rate is 0.5 mL/min; the column temperature is 30 ℃; sample introduction amount: 5 mu L of the solution; changing the detection wavelength: 190-400 nm;
s4, obtaining the linear equation, correlation coefficient and detection limit of acrylamide under the experiment of step S2:
s41, accurately weighing an acrylamide standard substance with the purity of 99.9 percent into a 50mL volumetric flask, dissolving, diluting and fixing the volume by using ultrapure water, and preparing an acrylamide standard solution with the concentration of 1000 mu g/mL; then taking a proper amount of acrylamide standard solution, diluting with ultrapure water, fixing the volume, and preparing into 100 mu g/mL acrylamide standard use solution;
s42, respectively taking 100 mu g/mL acrylamide standard use solution into blank ultrapure water, diluting step by step to prepare serial standard working solutions with mass concentrations of 0.05 mu g/mL, 0.10 mu g/mL, 0.50 mu g/mL, 1.00 mu g/mL and 5.00 mu g/mL;
please refer to fig. 1, which is a diagram illustrating a calibration curve of acrylamide;
s43, analyzing the mixture sequentially from low concentration to high concentration by a liquid chromatograph, determining the qualitative retention time and the quantitative peak area to obtain a linear equation and a correlation coefficient of the mixture;
FIG. 2 is a schematic diagram of a liquid chromatogram showing acrylamide concentration of 1.0. mu.g/mL;
s44, calculation of acrylamide detection limit: adding 40 mu L of acrylamide standard solution with the concentration of 10 mu g/mL into 10g of treated quartz sand (replacing a blank soil sample), performing ultrasonic extraction for 30min by using 20mL of ultrapure water, centrifuging, taking supernate to be tested, repeatedly measuring for 7 times according to a test method, calculating the standard deviation S of the measured value, and calculating the detection limit of the soil sample by using 3 times of standard deviation:
wherein, the calculation formula of the detection limit is as follows: MDL ═ t(n-1,0.99)*S，
Wherein, MDL-method detection limit;
t-degree of freedom is (n-1), and t distribution with a confidence of 99% is (n-7, t-3.143);
s-standard deviation of n replicates;
n-the number of replicates of the sample;
wherein, the method detection limit for determining the soil acrylamide according to the technical guide of revision of environmental detection and analysis method Standard (HJ 168-: 0.02 mg/kg;
wherein, the quartz sand is used for simulating the cleanest soil environment and replacing a blank soil sample;
s5, under the experimental conditions of the step S2, the carclazyte soil sample is subjected to labeling: after acrylamide is added into the blank soil sample, measuring for 6 times according to the whole sequence of the step S2, and measuring the precision and the accuracy of the blank soil sample after the standard addition;
wherein, the blank soil samples are respectively added with the standard and then measured for 6 times according to the whole procedure of the standard method steps, and the measurement result of the blank soil added with the standard is shown in the table 1:
TABLE 1 precision and accuracy results for blank soil spiking
As can be seen from Table 1, the relative standard deviations of the measurement results of the acrylamide standard-added samples in the blank soil samples are respectively 4.8% and 5.7%, the average standard-added recovery rates are respectively 91.1% and 92.5%, and the blank standard-added results meet the quality control requirements of the analysis and test.
S6, labeling the treated mealy clay under the experimental conditions of step S2: and (4) after the powdery clay sample is taken and added with acrylamide, measuring for 6 times according to the whole procedure of the step S2, and measuring the precision and the accuracy of the powdery clay sample after the standard addition.
Wherein, the processed silty clay is adopted for standard test, the whole procedure is measured for 6 times according to the standard method, and the precision and accuracy test results of the sample after standard addition are shown in the table 2:
TABLE 2 precision and accuracy results for the addition of a silty clay target
| Sample matrix | Components | Background value/. mu.g | Plus scalar quantity/mug | Measured value/. mu.g | Average value/. mu.g | Average recovery rate/%) | RSD％ |
| Powdery clay | Acrylamide | 0.00 | 2.40 | 2.03，1.92，2.23，1.92，1.92，2.38 | 2.01 | 86.1 | 9.4 |
| Powdery clay | Acrylamide | 0.00 | 6.00 | 5.92，5.97，5.71，5.41，5.38，5.63 | 5.67 | 94.5 | 4.4 |
| Powdery clay | Acrylamide | 0.00 | 30.0 | 23.6，23.0，23.3，24.2，22.3，22.3 | 23.1 | 77.1 | 3.3 |
As can be seen from Table 2, the relative standard deviations of the acrylamide measurement results after the soil sample matrix is subjected to standard addition are respectively 9.4%, 4.4% and 3.3%, and the average standard addition recovery rates are 86.1%, 94.5% and 77.1%, which indicates that the method has good precision and accuracy, and the results meet the quality control requirements of the analysis and test.
FIG. 3 is a liquid chromatogram of acrylamide obtained by adding 2.40 μ g of standard substance to powdery clay;
the content of acrylamide in soil is determined by determining the conditions of a liquid chromatograph and establishing a high performance liquid chromatography method, and the result shows that:
the detection limit of acrylamide in soil measured by the method is 0.02mg/kg, the standard recovery rate of the silty clay sample is 77.1-99.5%, and the relative standard deviation is 3.3-9.4%;
the method has the advantages of rapidness, accuracy, short pretreatment time, low detection limit and the like, the extractant and the mobile phase are basically ultrapure water, the environmental pollution is less, the accuracy and the precision are better, and the method is suitable for the detection and analysis of acrylamide in soil.
Example two
The liquid chromatography experiment is carried out by controlling the ratio of different mobile phases, changing the flow rate and detecting the wavelength by a variable method so as to verify the optimal liquid chromatography condition:
in the implementation of step S3, the following three methods can be employed to control the liquid chromatography conditions under the variable method:
the first method comprises the following steps: fixing other liquid chromatography conditions unchanged: the flow rate is 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; changing the proportion of the mobile phase;
wherein, the proportions of the mobile phases are respectively methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90);
acrylamide has strong polarity and relatively weak retention on a reverse phase chromatographic column, pure water can be used as a mobile phase, but in order to protect the chromatographic column as much as possible, a certain proportion of an organic phase is added. The proportions of the mobile phases are respectively compared, and according to the experimental result, the ratio of the mobile phase to the mobile phase is as follows: acrylamide and interferents in a sample can achieve better separation degree under the condition of water (5: 95);
and the second method comprises the following steps: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; the flow rate was varied: 0.3-0.6 mL/min;
wherein, the flow rates are respectively 0.3mL/min, 0.4mL/min, 0.5mL/min and 0.6mL/min, and the result shows that when the flow rate is set to be 0.5mL/min, the peak shape is better and the resolution is better;
and the third is that: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the flow rate is 0.5 mL/min; the column temperature is 30 ℃; sample introduction amount: 5 mu L of the solution; changing the detection wavelength: 190-400 nm;
wherein the detection wavelengths are 190nm, 200nm and 210nm respectively; scanning standard solution of acrylamide by using DAD spectrum, and according to the scanning result of the standard solution of acrylamide in the wavelength range of 190-400nm, please refer to FIG. 4, the strong absorption peak of acrylamide is at 190-200 nm, and 210nm is selected as the detection wavelength of acrylamide considering that the cut-off wavelengths of water and methanol are 190nm and 210nm respectively.
Verification "mobile phase methanol: water (volume ratio 5: 95) with flow rate of 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 μ L "is the optimal liquid chromatography condition.
According to the technical scheme, after the soil sample is subjected to the steps of ultrasonic extraction, centrifugation, filtration and the like, the content of acrylamide in the soil is determined by adopting the high performance liquid chromatography, and the method has the characteristics of simplicity in operation, high sensitivity and good reproducibility, and can be used for rapidly and effectively determining the residual amount of acrylamide in the soil.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A detection method for detecting acrylamide in soil is characterized by comprising the following steps:
s1, sample pretreatment: accurately weighing 10.00g of soil sample in a 50mL polypropylene centrifuge tube with a cover, performing ultrasonic extraction for 30min by using 20mL ultrapure water, centrifuging for 3min at 8000r/min, and filtering supernate by using a 0.45-micrometer water system needle filter to be detected.
S2, detecting acrylamide in soil under the optimal liquid chromatograph conditions:
the chromatographic conditions are as follows: a chromatographic column: ZORBAX Eclipse Plus C18 column (4.6X 100mm, 3.5 μm); mobile phase methanol: water (volume ratio 5: 95) with flow rate of 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 μ L.
S3, carrying out chromatographic separation experiments under the conditions of different mobile phase proportions, flow rate change and detection wavelength by controlling a variable method to verify the optimal liquid chromatographic condition, wherein the liquid chromatographic condition under the control of the variable method can adopt the following three methods:
the first method comprises the following steps: fixing other liquid chromatography conditions unchanged: the flow rate is 0.5 mL/min; the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; changing the mobile phase: methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90);
and the second method comprises the following steps: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the column temperature is 30 ℃; the detection wavelength is 210 nm; sample introduction amount: 5 mu L of the solution; the flow rate was varied: 0.3-0.6 mL/min;
and the third is that: fixing other liquid chromatography conditions unchanged: mobile phase methanol: water (volume ratio 5: 95); the flow rate is 0.5 mL/min; the column temperature is 30 ℃; sample introduction amount: 5 mu L of the solution; changing the detection wavelength: 190-400 nm;
s4, obtaining the linear equation, correlation coefficient and detection limit of acrylamide under the experiment of step S2:
s41, accurately weighing an acrylamide standard substance with the purity of 99.9 percent into a 50mL volumetric flask, dissolving, diluting and fixing the volume by using ultrapure water, and preparing an acrylamide standard solution with the concentration of 1000 mu g/mL; then taking a proper amount of acrylamide standard solution, diluting with ultrapure water, fixing the volume, and preparing into 100 mu g/mL acrylamide standard use solution;
s42, respectively taking 100 mu g/mL acrylamide standard use solution into blank ultrapure water, diluting step by step to prepare serial standard working solutions with mass concentrations of 0.05 mu g/mL, 0.10 mu g/mL, 0.50 mu g/mL, 1.00 mu g/mL and 5.00 mu g/mL;
s43, analyzing the mixture sequentially from low concentration to high concentration by a liquid chromatograph, determining the qualitative retention time and the quantitative peak area to obtain a linear equation and a correlation coefficient of the mixture;
s44, calculation of acrylamide detection limit: adding 40 mu L of acrylamide standard solution with the concentration of 10 mu g/mL into 10g of treated quartz sand (replacing a blank soil sample), performing ultrasonic extraction for 30min by using 20mL of ultrapure water, centrifuging, taking supernate to be tested, repeatedly measuring for 7 times according to a test method, calculating the standard deviation S of the measured value, and calculating the detection limit of the soil sample by using 3 times of standard deviation:
wherein, the calculation formula of the detection limit is as follows: MDL ═ t(n-1,0.99)*S，
Wherein, MDL-method detection limit;
t-degree of freedom is (n-1), and t distribution with a confidence of 99% is (n-7, t-3.143);
s-standard deviation of n replicates;
n-the number of replicates of the sample;
s5, under the experimental conditions of the step S2, the carclazyte soil sample is subjected to labeling: after acrylamide is added into the blank soil sample, measuring for 6 times according to the whole sequence of the step S2, and measuring the precision and the accuracy of the blank soil sample after the standard addition;
s6, labeling the treated mealy clay under the experimental conditions of step S2: and (4) after the powdery clay sample is taken and added with acrylamide, measuring for 6 times according to the whole procedure of the step S2, and measuring the precision and the accuracy of the powdery clay sample after the standard addition.
2. The method as claimed in claim 1, wherein in step S3, the first flowing phase ratio under the controlled variable method is methanol: water (10: 90); methanol: water (5: 95); acetonitrile: water (5: 90); acetonitrile: water (10: 90).
3. The method as claimed in claim 1, wherein in step S3, the second flow rate is 0.3mL/min, 0.4mL/min, 0.5mL/min, or 0.6mL/min under the control variable method.
4. The method as claimed in claim 1, wherein in step S3, the third detection wavelengths in the controlled variable method are 190nm, 200nm and 210nm, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110493403.4A CN113203812A (en) | 2021-05-07 | 2021-05-07 | Detection method for determining acrylamide in soil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110493403.4A CN113203812A (en) | 2021-05-07 | 2021-05-07 | Detection method for determining acrylamide in soil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113203812A true CN113203812A (en) | 2021-08-03 |
Family
ID=77030176
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110493403.4A Pending CN113203812A (en) | 2021-05-07 | 2021-05-07 | Detection method for determining acrylamide in soil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113203812A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2625499A1 (en) * | 2005-09-27 | 2007-04-05 | Lance Liotta | Method of isolating analytes from a sample |
| CN102749411A (en) * | 2012-07-11 | 2012-10-24 | 中国烟草总公司郑州烟草研究院 | Determination method for acrylamide in main stream smoke of cigarette |
| CN104297398A (en) * | 2013-07-16 | 2015-01-21 | 广东省东莞市质量监督检测中心 | A detection method of acrylamide monomer content in paper and paper products |
| EP2842614A1 (en) * | 2013-08-30 | 2015-03-04 | Biotage AB | Sample preparation method for analysis of acrylamide |
| CN110208439A (en) * | 2019-07-16 | 2019-09-06 | 中国热带农业科学院农产品加工研究所 | A kind of rapid detection method of acrylamide |
-
2021
- 2021-05-07 CN CN202110493403.4A patent/CN113203812A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2625499A1 (en) * | 2005-09-27 | 2007-04-05 | Lance Liotta | Method of isolating analytes from a sample |
| CN102749411A (en) * | 2012-07-11 | 2012-10-24 | 中国烟草总公司郑州烟草研究院 | Determination method for acrylamide in main stream smoke of cigarette |
| CN104297398A (en) * | 2013-07-16 | 2015-01-21 | 广东省东莞市质量监督检测中心 | A detection method of acrylamide monomer content in paper and paper products |
| EP2842614A1 (en) * | 2013-08-30 | 2015-03-04 | Biotage AB | Sample preparation method for analysis of acrylamide |
| CN110208439A (en) * | 2019-07-16 | 2019-09-06 | 中国热带农业科学院农产品加工研究所 | A kind of rapid detection method of acrylamide |
Non-Patent Citations (7)
| Title |
|---|
| SHELDON S 等: "Degradation and Leaching of Acrylamide in soil", 《JOURNAL OF ENVIRONMENTAL QUALITY》 * |
| 中国检验检疫科学研究院 等: "玩具中丙烯酰胺的测定", 《中华人民共和国出入境检验检疫行业标准 SN/T 2401-2009》 * |
| 刘成霞 等: "高效液相色谱法测定土壤中己内酰胺", 《广东化工》 * |
| 孙真 等: "高效液相色谱法测定油炸鸡腿中丙烯酰胺的含量", 《食品工业科技》 * |
| 张丽 等 中国医药科技出版社 * |
| 李振球 等: "高效液相色谱测定燃香中丙烯酰胺的研究", 《中国检验检测》 * |
| 魏恩棋 等: "《环境介质中硝基芳烃类化合物分析测试技术》", 31 December 2015, 天津大学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Du et al. | An in situ immobilized pipette tip solid phase microextraction method based on molecularly imprinted polymer monolith for the selective determination of difenoconazole in tap water and grape juice | |
| Pebdani et al. | Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry | |
| Yan et al. | Simultaneous determination of four phthalate esters in bottled water using ultrasound-assisted dispersive liquid–liquid microextraction followed by GC-FID detection | |
| CN103884785B (en) | A kind of detection method of selenium | |
| Zhou et al. | Ionic liquid for improved single-drop microextraction of aromatic amines in water samples | |
| Hu et al. | Simultaneous determination of palladium, platinum, rhodium and gold by on-line solid phase extraction and high performance liquid chromatography with 5-(2-hydroxy-5-nitrophenylazo) thiorhodanine as pre-column derivatization regents | |
| CN109696499B (en) | A highly sensitive method for the determination of nitrosamines in water based on high-resolution mass spectrometry | |
| Zhang et al. | A disposable molecularly imprinted sensor based on Graphe@ AuNPs modified screen-printed electrode for highly selective and sensitive detection of cyhexatin in pear samples | |
| CN106290670A (en) | A kind of method of column front derivation chromatogram ration analysis perfluorocarboxylic acid compound | |
| CN102435703A (en) | Method for simultaneously detecting multiple microcystins in water | |
| Xu et al. | Preparation of a hydrophilic molecularly imprinted polymer and its application in solid-phase extraction to determine of trace acrylamide in foods coupled with high-performance liquid chromatography | |
| CN112684070B (en) | A method for determining semi-volatile organic compounds in solid waste | |
| Zhang et al. | Porous boronate affinity monolith for on-line extraction coupled to high-performance liquid chromatography for sensitive analysis of heterocyclic aromatic amines in food samples | |
| CN112684069A (en) | Method for measuring methylnaphthalene compound in water | |
| CN113203812A (en) | Detection method for determining acrylamide in soil | |
| CN104251827A (en) | Method for determining concentration of mercury ions or silver ions in solution | |
| CN111707770B (en) | Method for measuring isoprene content in butyl rubber liquid by gas chromatography internal standard method | |
| CN115963204B (en) | Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by utilizing ultra-high liquid chromatography | |
| Li et al. | Identification of 3-chloro-1, 2-propandiol using molecularly imprinted composite solid-phase extraction materials | |
| Sun et al. | Determination of chromium (III) and total chromium in water by derivative atomic absorption spectrometry using flow injection on-line preconcentration with a double microcolumn | |
| CN108956812B (en) | Method for detecting water-soluble organic chloride pesticide residue in soil | |
| CN108872416B (en) | Method for simultaneously and quantitatively detecting erucamide and ethylene bis-stearamide | |
| Mirmoghaddam et al. | Application of response surface modeling for optimization and determination of malondialdialdehyde by vortex-assisted dispersive liquid-liquid microextraction and GC-FID | |
| Yan et al. | Further investigation of array capillary in-tube solid-phase microextraction of trace organic pollutants in water samples | |
| Zanjani et al. | Analysis of n-alkanes in water samples by means of headspace solvent microextraction and gas chromatography |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |