CN115963204A - Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography - Google Patents

Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography Download PDF

Info

Publication number
CN115963204A
CN115963204A CN202211740388.XA CN202211740388A CN115963204A CN 115963204 A CN115963204 A CN 115963204A CN 202211740388 A CN202211740388 A CN 202211740388A CN 115963204 A CN115963204 A CN 115963204A
Authority
CN
China
Prior art keywords
difluorobenzaldehyde
amino
culture medium
liquid chromatography
water
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
Application number
CN202211740388.XA
Other languages
Chinese (zh)
Inventor
毛建霏
杨迪
安孝思
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guizhou Jian'ande Technology Co ltd
Original Assignee
Guizhou Jian'ande Technology Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guizhou Jian'ande Technology Co ltd filed Critical Guizhou Jian'ande Technology Co ltd
Priority to CN202211740388.XA priority Critical patent/CN115963204A/en
Publication of CN115963204A publication Critical patent/CN115963204A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/80Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in fisheries management

Landscapes

  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)

Abstract

The invention discloses a method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography, which adopts an AgilentInfinityIIPrime1260 ultra-high liquid chromatography and a VWD detector, uses a Shim-packGISTC18, a 250mm multiplied by 4.6mm, and a 5 mu m chromatographic column, and uses 0.1% phosphoric acid aqueous solution and acetonitrile as flowing phase to detect the 2-amino-3, 4-difluorobenzaldehyde. The 2-amino-3, 4-difluorobenzaldehyde has good linear relation in the range of 0.500 mg/L-10.0 mg/L, the linear equation is y =90.74x +1.16, and the linear correlation coefficient R 2 =0.9998; LOD of 2-amino-3, 4-difluorobenzaldehyde in test water was 0.0108mg/L and LOQ was0.0359mg/L; LOD in the algae culture medium is 0.0100mg/L, LOQ is 0.0334mg/L, and the detection of trace sample concentration can be met; the detection method has the characteristics of strong specificity, high accuracy, short peak-producing time, good reproducibility, simple operation and the like.

Description

Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography
Technical Field
The invention belongs to the technical field of organic compound detection, and particularly relates to a method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using an ultra-high liquid chromatography.
Background
2-amino-3, 4-difluorobenzaldehyde (FDFA) with CAS number of 1602097-79-9 and molecular formula C 7 H 5 F 2 NO, molecular weight 157.1, structural formula:
Figure BDA0004031982130000011
2-amino-3, 4-difluorobenzaldehyde is an important chemical raw material and is widely used as a pesticide intermediate. At present, the related reports of 2-amino-3, 4-difluorobenzaldehyde are less, and no quality control method related to 2-amino-3, 4-difluorobenzaldehyde is disclosed, so that the establishment of the detection method of 2-amino-3, 4-difluorobenzaldehyde is very important for industrial application and quality control in the application process.
Disclosure of Invention
The invention aims to provide a method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography, which realizes the quality control of the 2-amino-3, 4-difluorobenzaldehyde.
The purpose of the invention is achieved by the following technical scheme:
a method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography comprises the following steps: and (1) drawing a standard curve: accurately weighing 0.05015g of 2-amino-3, 4-difluorobenzaldehyde standard substance in a 50mL volumetric flask, dissolving and diluting the standard substance to a scale by using acetonitrile, shaking the solution to prepare a standard stock solution of the 2-amino-3, 4-difluorobenzaldehyde with the concentration of 1000mg/L, taking a proper amount of standard stock solution, diluting the standard stock solution into a series of standard working solutions with the concentration of 0.500-10.0 mg/L by using the acetonitrile, measuring the peak area by using a solvent as a blank control according to the condition of ultra-high liquid chromatography, and drawing a standard curve to obtain a linear regression equation; and (2) preparing a test solution: accurately weighing 1.30371g of 2-amino-3, 4-difluorobenzaldehyde sample in a 25mL volumetric flask respectively, dissolving with acetonitrile, fixing the volume to a scale, shaking up, and preparing to obtain a stock solution of the 2-amino-3, 4-difluorobenzaldehyde sample with the concentration of 52003 mg/L; respectively sucking a proper amount of sample stock solution into two 100mL volumetric flasks, respectively diluting with test water and an algae culture medium to obtain a test solution to be tested, and testing by ultra-high liquid chromatography; (3) measurement of test article: setting the operating conditions of an ultrahigh liquid chromatography instrument, carrying out ultrahigh liquid chromatography determination on the sample solution after the instrument is stable, and calculating the content of the 2-amino-3, 4-difluorobenzaldehyde in the sample solution according to a linear regression equation.
In the step (1), the concentrations of the series of standard working solutions are respectively 0.500mg/L, 1.00mg/L, 2.00mg/L, 4.00mg/L, 8.00mg/L and 10.0mg/L.
The ultra-high liquid chromatogram adopts an Agilent Infinity II Prime1260 chromatograph, and the instrument operation conditions of the ultra-high liquid chromatogram are as follows: a chromatographic column: shim-pack GIST C18, 250 mm. Times.4.6 mm,5 μm; sample introduction volume: 2.0-8.0 mu L; flow rate: 0.4-0.80 mL/min; detection wavelength: 218-223 nm; mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; column temperature: 32 to 38 ℃.
Preferably, the injection volume is 5.00. Mu.L.
Preferably, the flow rate is 0.60mL/min.
Preferably, the detection wavelength is 221nm.
Preferably, the volume ratio of mobile phases a and B is 30.
Preferably, the column temperature is 35 ℃.
The linear regression equation of the invention is y =90.74x +1.16, and the linear correlation coefficient R 2 Is 0.9998.
The LOD of the invention in test water is 0.0108mg/L, and the LOQ is 0.0359mg/L; LOD in the algal culture medium was 0.0100mg/L and LOQ was 0.0334mg/L.
The invention has the beneficial effects that:
1. the invention provides a method for detecting 2-amino-3, 4-difluorobenzaldehyde for the first time by using an ultrahigh liquid chromatography, and provides technical references for the subsequent production and application process of the 2-amino-3, 4-difluorobenzaldehyde and the quality control in related researches.
2、The invention is examined by linear test, the linear relation is good in the range of 0.500 mg/L-10.0 mg/L, the linear equation is y =90.74x +1.16, and the linear correlation coefficient R 2 =0.9998。
3. In the specificity test, by comparing spectrograms of a test water and a blank sample of an algae culture medium and a sample with a recovery rate, the 2-amino-3, 4-difluorobenzaldehyde peaks at 6.9min, and the blank sample has no interference peak at the time point, so that the specificity is good.
4. According to detection limit and quantitative limit tests, the LOD of the 2-amino-3, 4-difluorobenzaldehyde in test water is 0.0108mg/L, and the LOQ is 0.0359mg/L; the LOD in the algae culture medium is 0.0100mg/L, the LOQ is 0.0334mg/L, and the detection of the concentration of a trace sample can be met.
5. The recovery rate and the repeatability test result show that the average addition recovery rates of 2-amino-3, 4-difluorobenzaldehyde with different concentrations in test water are respectively 87.7% and 97.1%, and the relative standard deviations of the recovery rates are respectively 4.28% and 0.201%; the average adding recovery rates of 2 types of 2-amino-3, 4-difluorobenzaldehyde with different concentrations in the algae culture medium are respectively 92.2% and 102%, and the relative standard deviations of the recovery rates are respectively 3.89% and 0.164%.
Drawings
FIG. 1 is a graph of a linear fit of 2-amino-3, 4-difluorobenzaldehyde in acetonitrile;
FIG. 2 shows a typical pattern (4.00 mg/L) for 2-amino-3, 4-difluorobenzaldehyde;
FIG. 3 is a blank spectrum of test water;
FIG. 4 is a blank map of an algae culture medium;
FIG. 5 is a typical spectrum of a low concentration recovery spiked solution in 2-amino-3, 4-difluorobenzaldehyde test water;
FIG. 6 is a typical spectrum of a high concentration recovery spiked solution in 2-amino-3, 4-difluorobenzaldehyde test water;
FIG. 7 is a typical chromatogram of the spiked solution for low concentration recovery in 2-amino-3, 4-difluorobenzaldehyde algal culture medium;
FIG. 8 is a typical spectrum of a spiked solution for high recovery of 2-amino-3, 4-difluorobenzaldehyde algal culture medium.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the scope of the invention.
The methods, starting materials, reagents or apparatus of the invention are generally prepared by conventional methods or are commercially available, unless otherwise specified.
The following examples employ reagents and instruments including, but not limited to:
1. reagents and solvents
(1) Acetonitrile: HPLC grade, shanghai' an spectrum experiment science & technology GmbH;
(2) Phosphoric acid: HPLC grade, honeywell (china) ltd;
(3) UP water: resistivity, 18.2M Ω cm;
(4) Test water: self-made in a laboratory;
(5) Algae culture medium: self-made in a laboratory;
(6) 2-amino-3, 4-difluorobenzaldehyde standard product with the purity of 99.72194%:
2. main instrument equipment
(1) Ultra-high performance liquid chromatograph: agilent Infinity II Prime1260, VWD detector;
(2) And (3) chromatographic column: shim-pack GIST C18, 250 mm. Times.4.6 mm,5 μm;
(3) An electronic balance: METTLER TOLEDO, XS105, HFC0044;
example 1:
(1) Drawing a standard curve: accurately weighing 0.05015g of 2-amino-3, 4-difluorobenzaldehyde standard substance in a 50mL volumetric flask, dissolving and diluting the standard substance to a scale by using acetonitrile, shaking the standard substance to prepare a standard stock solution of the 2-amino-3, 4-difluorobenzaldehyde with the concentration of 1000mg/L, taking a proper amount of standard stock solution, diluting the standard stock solution by using the acetonitrile into a series of standard working solutions with the concentrations of 0.500mg/L, 1.00mg/L, 2.00mg/L, 4.00mg/L, 8.00mg/L and 10.0mg/L respectively, measuring the peak area by using the solvent as a blank control according to the condition of ultra-high liquid chromatography, and drawing a standard curve to obtain a linear regression equation;
(2) Preparing a test solution: accurately weighing 1.30371g of 2-amino-3, 4-difluorobenzaldehyde sample in a 25mL volumetric flask respectively, dissolving with acetonitrile, fixing the volume to a scale, shaking up, and preparing to obtain a stock solution of the 2-amino-3, 4-difluorobenzaldehyde sample with the concentration of 52003 mg/L; respectively sucking a proper amount of sample stock solution into two 100mL volumetric flasks, respectively diluting with test water and an algae culture medium to obtain a test solution to be tested, and testing by ultra-high liquid chromatography;
(3) And (3) testing the test sample: setting the operating conditions of an ultra-high liquid chromatography instrument, after the instrument is stabilized, carrying out ultra-high liquid chromatography determination on the test solution, and calculating the content of the 2-amino-3, 4-difluorobenzaldehyde in the test solution according to a linear regression equation.
The operating conditions of the instrument for the ultra-high liquid chromatography of the embodiment are as follows: an Agilent Infinity IIPrime1260 chromatograph is adopted, a chromatographic column is Shim-pack GIST C18, the specification is 250mm multiplied by 4.6mm, and the size is 5 mu m; the sample injection volume is 5.0 mu L; the flow rate is 0.6mL/min; the detection wavelength is 221nm; mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile, the volume ratio of mobile phase A and B is 30; the column temperature was 35 ℃.
Example 2:
(1) Drawing a standard curve: accurately weighing 0.05015g of 2-amino-3, 4-difluorobenzaldehyde standard substance in a 50mL volumetric flask, dissolving and diluting the standard substance to a scale by using acetonitrile, shaking the standard substance to prepare a standard stock solution of the 2-amino-3, 4-difluorobenzaldehyde with the concentration of 1000mg/L, taking a proper amount of standard stock solution, diluting the standard stock solution by using the acetonitrile into a series of standard working solutions with the concentrations of 0.500mg/L, 1.00mg/L, 2.00mg/L, 4.00mg/L, 8.00mg/L and 10.0mg/L respectively, measuring the peak area by using the solvent as a blank control according to the condition of ultra-high liquid chromatography, and drawing a standard curve to obtain a linear regression equation;
(2) Preparing a test solution: respectively and precisely weighing 1.30371g of 2-amino-3, 4-difluorobenzaldehyde sample in a 25mL volumetric flask, dissolving with acetonitrile, fixing the volume to a scale, shaking up, and preparing to obtain a stock solution of the 2-amino-3, 4-difluorobenzaldehyde sample with the concentration of 52003 mg/L; respectively sucking a proper amount of sample stock solution into two 100mL volumetric flasks, respectively diluting with test water and an algae culture medium to obtain a test solution to be tested, and testing by ultra-high liquid chromatography;
(3) And (3) testing the test sample: setting the operating conditions of an ultrahigh liquid chromatography instrument, carrying out ultrahigh liquid chromatography determination on the sample solution after the instrument is stable, and calculating the content of the 2-amino-3, 4-difluorobenzaldehyde in the sample solution according to a linear regression equation.
The operating conditions of the instrument for the ultra-high liquid chromatography of the embodiment are as follows: an Agilent Infinity IIPrime1260 chromatograph is adopted, and a chromatographic column is Shim-pack GIST C18, the specification is 250mm multiplied by 4.6mm, and the size is 5 mu m; the sample injection volume is 2.0 mu L; the flow rate is 0.4mL/min; the detection wavelength is 218nm; mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile, the volume ratio of mobile phase A and B is 30; the column temperature was 32 ℃.
Example 3:
(1) Drawing a standard curve: accurately weighing 0.05015g of 2-amino-3, 4-difluorobenzaldehyde standard substance in a 50mL volumetric flask, dissolving and diluting the standard substance to a scale by using acetonitrile, shaking the standard substance to prepare a standard stock solution of the 2-amino-3, 4-difluorobenzaldehyde with the concentration of 1000mg/L, taking a proper amount of standard stock solution, diluting the standard stock solution by using the acetonitrile into a series of standard working solutions with the concentrations of 0.500mg/L, 1.00mg/L, 2.00mg/L, 4.00mg/L, 8.00mg/L and 10.0mg/L respectively, measuring the peak area by using the solvent as a blank control according to the condition of ultra-high liquid chromatography, and drawing a standard curve to obtain a linear regression equation;
(2) Preparing a test solution: accurately weighing 1.30371g of 2-amino-3, 4-difluorobenzaldehyde sample in a 25mL volumetric flask respectively, dissolving with acetonitrile, fixing the volume to a scale, shaking up, and preparing to obtain a stock solution of the 2-amino-3, 4-difluorobenzaldehyde sample with the concentration of 52003 mg/L; respectively sucking a proper amount of sample stock solution into two 100mL volumetric flasks, respectively diluting with test water and an algae culture medium to obtain a test solution to be tested, and testing by ultra-high liquid chromatography;
(3) And (3) testing the test sample: setting the operating conditions of an ultra-high liquid chromatography instrument, after the instrument is stabilized, carrying out ultra-high liquid chromatography determination on the test solution, and calculating the content of the 2-amino-3, 4-difluorobenzaldehyde in the test solution according to a linear regression equation.
The operating conditions of the instrument for the ultra-high liquid chromatography of the embodiment are as follows: an Agilent Infinity IIPrime1260 chromatograph is adopted, and a chromatographic column is Shim-pack GIST C18, the specification is 250mm multiplied by 4.6mm, and the size is 5 mu m; the sample injection volume is 8.0 mu L; the flow rate is 0.8mL/min; the detection wavelength is 223nm; mobile phase: a is 0.1% phosphoric acid aqueous solution, B is acetonitrile, the volume ratio of mobile phase A and B is 30; the column temperature was 38 ℃.
To further verify the feasibility of the present invention, the inventors carried out a series of methodological validation studies, some of which were summarized below:
1. linear investigation test
Absorbing the series of standard working solutions in the example 1, measuring according to the condition of the ultra-high liquid chromatography, and carrying out parallel sample injection for 2 times at each concentration, wherein the results are shown in a table 1; and drawing a standard curve by taking the average value of the concentration of the target as an abscissa and the average value of the peak area of the target as an ordinate.
Table 1: analysis results of 2-amino-3, 4-difluorobenzaldehyde (FDFA) standard working solution
Figure BDA0004031982130000061
The results showed that there was a linear relationship between y and x when the concentration of 2-amino-3, 4-difluorobenzaldehyde was in the range of 0.500mg/L to 10.0mg/L. Linear regression is carried out on the curve to obtain the equation of the tested substance in acetonitrile, wherein the equation is y =90.74x +1.16, and the linear correlation coefficient R 2 It was 0.9998 and the linear fit curve is shown in FIG. 1.
2. Specificity test
According to the ultra-high liquid chromatography condition, a test water blank sample, a test water recovery rate sample, an algae culture medium blank sample and an algae culture medium recovery rate sample are measured, and chromatograms of the blank sample and the recovery rate sample are compared. The retention time of the 2-amino-3, 4-difluorobenzaldehyde is 6.9min, and a blank sample has no interference peak at the time point, so that the result shows that the method has good specificity on the 2-amino-3, 4-difluorobenzaldehyde (FDFA).
3. Recovery and repeatability tests
(1) Test water recovery concentration preparation
Preparing and sucking 0.800mL of 2-amino-3, 4-difluorobenzaldehyde standard stock solution with the concentration of 100mg/L into a 100mL volumetric flask, dissolving with test water, fixing the volume to a scale, and shaking up to obtain the test solution with the test water low-concentration recovery rate with the concentration of 0.800 mg/L. The above procedure was repeated to prepare 5 replicates.
Preparing and sucking 0.230mL of 2-amino-3, 4-difluorobenzaldehyde standard stock solution with the concentration of 52003mg/L into a 100mL volumetric flask, dissolving with test water, fixing the volume to a scale, shaking up to obtain a test solution with the concentration of 120mg/L for the high-concentration recovery rate of test water, and repeating the operations to prepare 5 parallels.
Taking blank matrix and test water high and low concentration recovery rate test solution, diluting the high concentration recovery rate test solution by 20 times with acetonitrile, directly sampling the low concentration recovery rate test solution, filtering with 0.45 μm filter membrane, testing according to the operation conditions of the ultra-high liquid chromatography instrument, calculating the recovery rate according to formula (1), and calculating the Relative Standard Deviation (RSD) of the recovery rate according to formula (2) and formula (3).
(2) Preparation of recovery rate and concentration of algae culture medium
Preparing and sucking 0.800mL of 2-amino-3, 4-difluorobenzaldehyde standard stock solution with the concentration of 100mg/L into a 100mL volumetric flask, dissolving with an algae culture medium, fixing the volume to a scale, and shaking up to obtain the algae culture medium high-concentration recovery rate test solution with the concentration of 0.800 mg/L. The above procedure was repeated to prepare 5 replicates.
Preparing and sucking 1.000mL of 2-amino-3, 4-difluorobenzaldehyde standard stock solution with the concentration of 52003mg/L into a 100mL volumetric flask, dissolving with an algae culture medium, fixing the volume to a scale, shaking up to obtain a low-concentration recovery test solution of the algae culture medium with the concentration of 520mg/L, and repeating the operations to prepare 5 parallels.
Taking a blank matrix and a test solution of high and low concentration of the recovery rate of the algae culture medium, diluting the test solution of high concentration recovery rate by 100 times with acetonitrile, directly sampling the test solution of low concentration recovery rate, filtering the sample with a 0.45 mu m filter membrane, testing according to the operation conditions of an ultrahigh liquid chromatography instrument of the invention, calculating the recovery rate according to a formula (1), and calculating the Relative Standard Deviation (RSD) of the recovery rate according to a formula (2) and a formula (3).
Analytical methods precision is expressed in terms of reproducibility, expressed as the relative standard deviation RSD.
The reproducibility was analyzed using recovery test solutions and RSD was calculated at 5 levels for each of the high and low concentrations.
The analytical results are shown in tables 2 and 3,2, the average addition recoveries of 2-amino-3, 4-difluorobenzaldehyde (FDFA) in test water at different concentrations are 87.7% and 97.1%, respectively, and the relative standard deviations of the recoveries are 4.28% and 0.201%, respectively; the average addition recovery of 2 different concentrations of 2-amino-3, 4-difluorobenzaldehyde (FDFA) in algal culture medium was 92.2% and 102%, respectively, and the relative standard deviation of the recovery was 3.89% and 0.164%, respectively.
Figure BDA0004031982130000071
In the formula:
r-recovery,%;
cd is the actually measured concentration of a target substance, mg/L;
ca-target Physics addition concentration, mg/L.
Figure BDA0004031982130000081
In the formula:
s-standard deviation;
xi-recovery,%, from the ith measurement;
Figure BDA0004031982130000082
-average value of recovery,%;
n-the number of recovery rates involved in the calculation.
Figure BDA0004031982130000083
In the formula:
RSD-relative standard deviation,%.
Table 2: test results of recovery in test Water
Figure BDA0004031982130000084
Table 3: recovery in algal culture medium
Figure BDA0004031982130000085
Figure BDA0004031982130000091
4. Detection limit and quantification limit
The spectra obtained from the samples of the present invention with low recovery of concentration were analyzed and the results are shown in tables 4 and 5. At the concentration, the average signal-to-noise ratio (S/N) =223 of a target peak in test water and the average signal-to-noise ratio (S/N) =239 of the target peak in an algae culture medium; according to LOD =3 × assay concentration/(S/N), LOQ =10 × assay concentration/(S/N). The LOD of the method in test water is 0.0108mg/L; LOQ is 0.0359mg/L, LOD in the algae culture medium is 0.0100mg/L; LOQ is 0.0334mg/L.
Table 4: LOD and LOQ test results-test water
Figure BDA0004031982130000092
Table 5: LOD and LOQ test results-algae culture medium
Figure BDA0004031982130000093
Figure BDA0004031982130000101
While the invention has been described in detail in the foregoing by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that certain changes and modifications may be made therein based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography is characterized by comprising the following steps:
(1) Drawing a standard curve: accurately weighing 0.05015g of 2-amino-3, 4-difluorobenzaldehyde standard substance in a 50mL volumetric flask, dissolving and diluting the standard substance to a scale by using acetonitrile, shaking the solution to prepare a standard stock solution of the 2-amino-3, 4-difluorobenzaldehyde with the concentration of 1000mg/L, taking a proper amount of standard stock solution, diluting the standard stock solution into a series of standard working solutions with the concentration of 0.500-10.0 mg/L by using the acetonitrile, measuring the peak area by using a solvent as a blank control according to the condition of ultra-high liquid chromatography, and drawing a standard curve to obtain a linear regression equation;
(2) Preparing a test solution: accurately weighing 1.30371g of 2-amino-3, 4-difluorobenzaldehyde sample in a 25mL volumetric flask respectively, dissolving with acetonitrile, fixing the volume to a scale, shaking up, and preparing to obtain a stock solution of the 2-amino-3, 4-difluorobenzaldehyde sample with the concentration of 52003 mg/L; respectively sucking a proper amount of sample stock solution into two 100mL volumetric flasks, respectively diluting with test water and an algae culture medium to obtain a test solution to be tested, and testing by ultra-high liquid chromatography;
(3) And (3) testing the test sample: setting the operating conditions of an ultrahigh liquid chromatography instrument, carrying out ultrahigh liquid chromatography determination on the sample solution after the instrument is stable, and calculating the content of the 2-amino-3, 4-difluorobenzaldehyde in the sample solution according to a linear regression equation.
2. The method for detecting 2-amino-3, 4-difluorobenzaldehyde of water and algae culture medium according to claim 1, wherein the concentrations of the standard working solutions in step (1) are 0.500mg/L, 1.00mg/L, 2.00mg/L, 4.00mg/L, 8.00mg/L and 10.0mg/L, respectively.
3. The method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra high performance liquid chromatography as claimed in claim 1, wherein the ultra high performance liquid chromatography is performed by Agilent Infinity II Prime1260 chromatography, and the instrument operation conditions of the ultra high performance liquid chromatography are as follows: a chromatographic column: shim-pack GIST C18, 250 mm. Times.4.6 mm,5 μm; sample introduction volume: 2.0-8.0 mu L; flow rate: 0.4-0.80 mL/min; detection wavelength: 218-223 nm; mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; column temperature: 32 to 38 ℃.
4. The method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium according to claim 3, wherein the sample injection volume is 5.00 μ L.
5. The method of claim 3, wherein the flow rate is 0.60mL/min for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by ultra high performance liquid chromatography.
6. The method of claim 3, wherein the detection wavelength is 221nm for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by ultra-high performance liquid chromatography.
7. The method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium according to claim 3, wherein the volume ratio of the mobile phases A and B is 30.
8. The method of claim 3, wherein the column temperature is 35 ℃ for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by ultra high performance liquid chromatography.
9. The method of claim 1, wherein the step of performing ultra-high performance liquid chromatographyThe method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium is characterized in that in step (1), the linear regression equation is y =90.74x +1.16, and the linear correlation coefficient R is 2 Is 0.9998.
10. The method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algal culture medium according to claim 1, wherein the LOD of the method in the test water is 0.0108mg/L; LOQ is 0.0359mg/L, LOD in the algae culture medium is 0.0100mg/L; LOQ is 0.0334mg/L.
CN202211740388.XA 2022-12-30 2022-12-30 Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography Pending CN115963204A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211740388.XA CN115963204A (en) 2022-12-30 2022-12-30 Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211740388.XA CN115963204A (en) 2022-12-30 2022-12-30 Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography

Publications (1)

Publication Number Publication Date
CN115963204A true CN115963204A (en) 2023-04-14

Family

ID=87359728

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211740388.XA Pending CN115963204A (en) 2022-12-30 2022-12-30 Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography

Country Status (1)

Country Link
CN (1) CN115963204A (en)

Similar Documents

Publication Publication Date Title
Da Silva et al. Application of silica gel organofunctionalized with 3 (1-imidazolyl) propyl in an on-line preconcentration system for the determination of copper by FAAS
CN114019062B (en) Method for detecting related substances in rifampicin
CN113376305A (en) Solid-phase membrane extraction gas chromatography-mass spectrometry detection method for carbazole and polyhalogen carbazole in water body
CN108152425B (en) Method for detecting lignanoids in sesame oil by high performance liquid chromatography
CN107703222B (en) Method for determining trace organic amine in atmospheric particulates
CN111272900B (en) Gas chromatography analysis method for detecting content of 3-chloro-2, 2-dimethyl-1-propanol
CN112630365A (en) Method for determining content of dimyristoyl phosphatidylcholine by high performance liquid chromatography
CN115963204A (en) Method for detecting 2-amino-3, 4-difluorobenzaldehyde in water and algae culture medium by using ultra-high liquid chromatography
CN114217002B (en) Method for detecting contents of chamomile azulene and sabinene in chamomile essential oil
CN115684400A (en) HPLC detection method for ketoprofen ethyl ester in water and algae culture medium
CN113820409B (en) Method for detecting related substances in mother nucleus of moxifloxacin
CN112326856B (en) Method for rapidly detecting content of isothiazolinone compounds in water-based gloss oil
CN110895264A (en) Method for determining ethyl bromide in tenofovir alafenamide
CN111505163B (en) Method for detecting phenethyl methane sulfonate substances
CN108828101B (en) Method for determining diuron residues in sugarcane based on 3, 4-dichloroaniline
CN108195958B (en) Method for detecting N, N-diglycidyl-4-glycidyloxyaniline in plastic product
CN112461975A (en) Method for detecting coenzyme content in feed additive
CN114755332B (en) Method for detecting isomer impurities in p-fluorobenzonitrile by gas chromatography
CN116879428B (en) High performance liquid analysis method for residual content of phosphorylcholine in L-alpha-phosphorylcholine
CN112305100B (en) Method for detecting content of genotoxic impurity benzyl bromide in medicine
CN112730707B (en) Method for measuring content of nervonic acid by high performance liquid chromatography
CN116046518A (en) Method for detecting diethyl (3-pyridyl) -borane by ultra-high performance liquid chromatography
CN116223654A (en) HPLC-MS/MS detection method for 4-fluoro-N-isopropylaniline in soil and water
CN112730689B (en) Liquid chromatography analysis method of 2-amino-5, 8-dimethoxy [1,2,4] triazolo [1,5-c ] pyrimidine
CN109521120B (en) Quantitative determination of DNTF content by GC-AED independent calibration curve method (CIC method)

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