CN115684399A - High performance liquid detection and content determination method for chlorhydrin imine - Google Patents
High performance liquid detection and content determination method for chlorhydrin imine Download PDFInfo
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Abstract
The invention discloses a high performance liquid phase detection and content determination method of chlorohydrin imine, which adopts a ZORBAXSB-C18 chromatographic column and a PAD detector, takes 0.1 percent phosphoric acid solution and acetonitrile as mobile phases and quantifies by an external standard method. The chlorohydrin imine concentration of the invention isThe linear relation is good in the range of 0.05-1.00 mg/L, the linear equation is Y =128852X +787.02, and the linear correlation coefficient R 2 =0.9998. The LOD of the chlorohydrin imine in the method is 0.05mg/L, and the LOQ is 0.10mg/L. Target Peak RSD R.T. 0.04%, RSD Area Is 0.15%. The method has the characteristics of simple and convenient operation, rapidness, good separation effect, strong specificity, high precision and accuracy and the like.
Description
Technical Field
The invention belongs to the technical field of organic compound detection, and particularly relates to a high-performance liquid phase detection and content determination method of chlorohydrin imine.
Background
The chemical name of chlorhydrinidation is (2S) -1-chloro-3- [ [ (4-chlorophenyl) methylene]Amino group]-2-propanol of the formula C 10 H 11 Cl 2 NO, CAS registry number 1345879-87-9, having the following chemical formula:
the chlorhydrin imine is a chemical raw material, is commonly used as a medical intermediate, and has wide application prospect in the fields of pesticides, biological medicines, chemical industry and the like. The quality of chemical raw materials needs to be detected before production and application so as to ensure the application effect and the use safety of the chemical raw materials. At present, the qualitative and quantitative detection method of the chlorohydrin imine is not reported in the literature.
The invention establishes a quantitative and qualitative chlorhydrin imine detection method which is simple and convenient to operate, high-efficiency, good in separation degree, high in accuracy and strong in specificity by using a high performance liquid technology.
Disclosure of Invention
The invention aims to overcome the defect that the quality control technology of chlorohydrin imine in the prior art is still blank, and provides a high-performance liquid phase detection and content determination method of chlorohydrin imine.
The invention provides a high performance liquid phase detection and content determination method of chlorohydrin imine, which comprises the following detection steps: preparing a standard working solution: weighing a proper amount of chlorhydrin imine standard substance, adding a solvent to dissolve and dilute the standard substance to prepare a series of standard working solutions. (2) preparing a test solution: weighing a sample to be tested with a proper amount of chlorhydrin imine, adding a solvent to dissolve and dilute the sample to be tested to prepare a test solution. (3) measurement and calculation: injecting the blank solvent, the sample solution of chlorohydrin imine and the standard sample solution of chlorohydrin imine into a high performance liquid chromatograph for analysis, recording a chromatogram, and calculating the content of chlorohydrin imine in the sample solution according to an external standard method.
The solvent is acetonitrile, ultrapure water or n-octanol.
The high performance liquid chromatography adopts a ZORBAXSB-C18 chromatographic column and a PAD detector, and the analysis conditions of the high performance liquid chromatography are as follows:
sample introduction volume: 25-35 μ L;
flow rate: 0.8-1.5 mL/min;
mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; a: B =30 (v/v);
column temperature: 26 to 35 ℃;
detection wavelength: 250-260 nm.
Preferably, the sample introduction volume is 28-32 mu L, the flow rate is 1.0-1.2 mL/min, and the column temperature is 28-32 ℃.
Further preferably, the sample injection volume is 30 μ L, the flow rate is 1.0mL/min, and the column temperature is 30 ℃.
Preferably, the detection wavelength is 254nm.
Preferably, the concentration of the sample solution is 0.10 to 10.0mg/L.
Preferably, the concentration of the standard working solution is 0.05 to 10.00mg/L.
A high performance liquid phase detection and content determination method of chlorohydrin imine comprises the following specific steps:
(1) preparation of standard working solutions: accurately weighing 0.10025g of chlorohydrin imine standard substance in a 100mL volumetric flask, dissolving the chlorohydrin imine standard substance with acetonitrile to a constant volume to a scale, shaking up to obtain a standard mother solution with the concentration of 1002.5mg/L, putting 1.00mL of the standard mother solution in the 100mL volumetric flask, dissolving the standard mother solution with acetonitrile to a constant volume to a scale, shaking up to obtain a standard stock solution with the concentration of 10.00mg/L, and absorbing a proper amount of the standard stock solution to dilute the standard stock solution with acetonitrile to prepare a series of standard working solutions with the concentration of chlorohydrin imine of 0.05, 0.10, 0.20, 0.40, 0.60, 0.80 and 1.00mg/L.
(2) Preparation of a test solution: weighing 0.01-1.00 mg of chlorhydrin imine sample to be detected in a 100mL volumetric flask, using ultrapure water or n-octanol to perform constant volume to reach scales, and uniformly mixing to obtain chlorhydrin imine sample solution.
(3) Drawing a standard curve: and (3) sucking 25-35 mu L of the series of standard working solutions in the step (1) for HPLC determination, drawing a standard curve by taking the concentration of the series of standard working solutions as an abscissa and the peak area of the chlorohydrin imine as an ordinate, and solving a regression equation and a correlation coefficient.
(4) Sample determination and content calculation: and (3) sucking 25-35 mu L of the sample solution in the step (2) for HPLC measurement to obtain the peak area of the chlorhydrin imine in the sample, and substituting the peak area into the linear regression equation in the step (3) for calculation to obtain the concentration of the chlorhydrin imine in the sample.
The linear regression equation of the chlorohydrin imine is Y =128852X +787.02, and the linear correlation coefficient R 2 And the linear range is 0.05-1.00 mg/L, and the linear range is 0.9998.
The invention has the following beneficial effects:
1. the invention adopts LC2030CSDPlus high performance liquid chromatograph and uses ZORBAX SB-C 18 The invention can accurately detect the chlorohydrin imine in acetonitrile, ultrapure water and n-octanol by the chromatographic column and the PAD detector, and carry out content measurement on the chlorohydrin imine in the sample by an external standard method, thereby providing technical reference for quality control in the production and application process of the chlorohydrin imine and ensuring the quality to be controllable. The inventive chlorohydrin imine peaks at 4.3min, and a blank sample does not have an interference peak at this time point. The detection method has high efficiency, good target peak separation degree and low cost, and is suitable for qualitative and quantitative detection of the chlorohydrin imine in large-scale production and detection and analysis in laboratories.
2. The analytical method of the invention proves that the chemical test shows that: the linear relation of the chlorhydrin imine concentration is good in the range of 0.05-1.00 mg/L, the linear equation is Y =128852X +787.02, and the linear correlation coefficient R 2 =0.9998. The method has the detection limit LOD of 0.05mg/L and LOQ of 0.10mg/L on the chlorohydrin imine. Target Peak RSD R.T. 0.04%, RSD Area Is 0.15%. The recovery rate of the chlorhydrin imine in the ultrapure water is 94.4 to 98.3 percent, and the recovery rate of the chlorhydrin imine in the n-octanol is 90.0 to 98.9 percent. The method has the advantages of simple and convenient operation, rapidness, good separation effect, strong specificity, high precision, high accuracy and the like.
Drawings
FIG. 1 is a linear relationship diagram of chlorohydrin imine;
FIG. 2 is a typical map of chlorohydrin imine;
FIG. 3 is an acetonitrile blank spectrum;
FIG. 4 is a water blank spectrum;
FIG. 5 is an n-octanol blank map;
FIG. 6 is a typical profile (low concentration) of a water recovery spiked solution;
FIG. 7 is a typical profile (high concentration) of a water recovery spiked solution;
FIG. 8 is a typical profile (low concentration) of a spiked solution for n-octanol recovery;
FIG. 9 is a typical spectrum (high concentration) of a normalized solution of n-octanol recovery.
Detailed Description
The invention is further described below with reference to the drawings and examples, but is not limited to the scope of the invention.
The main instruments, main reagents and solutions used in the invention are as follows:
1. main instrument equipment
(1) High performance liquid chromatograph: LC2030CSDPlus;
(2) An electronic balance: mettler-tollido (china) ltd, model number: XSE105DU;
(3) Gas bath constant temperature oscillator: jiangsu Jintanhonghua instrument factory, model: ZD-85A, LHY190-1;
(4) Hunan instrument desk type high-speed centrifuge: hunan instruments laboratory Instrument development Co., ltd, model number: H1850.
2. primary reagents and solutions
(1) Phosphoric acid: super pure, tianjinkemi chemie ltd;
(2) Acetonitrile: HPLC, shanghai' an Spectrum Experimental science & technology GmbH;
(3) Ultrapure water: resistivity, 18.2M Ω cm.
Example 1:
the high performance liquid phase detection method of chlorohydrin imine in water includes the following steps:
(1) Preparation of standard working solutions: accurately weighing 0.10025g of chlorhydrin imine standard substance into a 100mL volumetric flask, dissolving with acetonitrile to constant volume to a scale, and shaking up to obtain a standard mother liquor with the concentration of 1002.5 mg/L; taking 1.00mL of standard mother liquor into a 100mL volumetric flask, dissolving with acetonitrile, fixing the volume to a scale, and shaking up to obtain a standard stock solution with the concentration of 10.00 mg/L; and (3) sucking a proper amount of standard stock solution, and diluting the stock solution with acetonitrile to prepare a series of standard working solutions with the concentration of chlorohydrin imine of 0.05, 0.10, 0.20, 0.40, 0.60, 0.80 and 1.00mg/L.
(2) Preparing a test solution: and (2) sucking 1.00mL of the standard sample stock solution with the concentration of 10.0mg/L in the step (1) into a 100mL volumetric flask, metering the volume to scale by using ultrapure water, and uniformly mixing to obtain a sample solution with the theoretical concentration of the chlorhydrin imine of 0.10mg/L.
(3) Drawing a standard curve: sucking 30 μ L of the series of standard working solutions in the step (1), injecting into a high performance liquid chromatograph for analysis, and obtaining the result shown in Table 1, wherein the concentration of the series of standard working solutions is used as a horizontal coordinate, the peak area of the chlorhydrin imine is used as a vertical coordinate, a standard curve is drawn, a regression equation and a correlation coefficient are obtained, and the linear regression equation of the chlorhydrin imine is
Y =128852X +787.02, linear correlation coefficient R2=0.9998, and the standard curve is shown in figure 1.
Table 1: test results of standard working solutions of the chlorohydrin imine series
(4) Measurement and sample content calculation: and (3) sucking 30 mu L of acetonitrile blank solvent, ultrapure water blank solvent and the sample solution in the step (2) and injecting the acetonitrile blank solvent, the ultrapure water blank solvent and the sample solution into a high performance liquid chromatograph for analysis to obtain the peak area of the chlorohydrin imine in the sample solution, and substituting the peak area into the linear regression equation for calculation to obtain the concentration of the chlorohydrin imine in the ultrapure water.
(5) The analysis conditions of the high performance liquid chromatography are as follows:
flow rate: 1.0mL/min;
mobile phase: a is 0.1% phosphoric acid aqueous solution, B is acetonitrile; a: B =30 (v/v);
column temperature: 30 ℃;
detection wavelength: 254nm.
Example 2:
a high performance liquid phase detection method of chlorohydrin imine in water.
Except for the concentration of the test sample in the step (2), other steps, conditions and reagent dosage are the same as those in the example 1.
The preparation method of the test solution comprises the following steps: and (2) sucking 1.00mL of the standard mother solution with the concentration of 1002.5mg/L in the step (1) into a 100mL volumetric flask, metering the volume to a scale by using ultrapure water, and uniformly mixing to obtain the sample solution with the theoretical concentration of the chlorhydrin imine of 10.0mg/L.
Example 3:
a high performance liquid phase detection method of chlorohydrin imine in water.
The absorption amount of the standard working solution, the acetonitrile blank solvent, the ultrapure water blank solvent and the sample solution in the step (2) is changed into 25 mu L, and the analysis conditions of the high performance liquid chromatography are changed into the following conditions: the flow rate was 0.8mL/min, the column temperature was 26 ℃ and the detection wavelength was 250nm, except that the other steps, conditions and the amount of reagents were the same as in example 1.
Example 4:
a high performance liquid phase detection method of chlorohydrin imine in water.
The absorption amount of the solution except the standard working solution, the acetonitrile blank solvent, the ultrapure water blank solvent and the sample solution in the step (2) is changed to 28 mu L, and the analysis conditions of the high performance liquid chromatography are changed to: the flow rate was 0.9mL/min, the column temperature was 28 ℃ and the detection wavelength was 252nm, and the other steps, conditions and amounts of reagents were the same as in example 1.
Example 5:
a high performance liquid phase detection method of chlorohydrin imine in water.
The absorption amount of the solution except the standard working solution, the acetonitrile blank solvent, the ultrapure water blank solvent and the sample solution in the step (2) is changed to 32 mu L, and the analysis conditions of the high performance liquid chromatography are changed to: the flow rate was 1.2mL/min, the column temperature was 32 ℃ and the detection wavelength was 256nm, and the other steps, conditions and reagent amounts were the same as in example 1.
Example 6:
a high performance liquid phase detection method of chlorohydrin imine in water.
The absorption amount of the standard working solution, the acetonitrile blank solvent, the ultrapure water blank solvent and the sample solution in the step (2) is changed into 35 mu L, and the analysis conditions of the high performance liquid chromatography are changed into the following conditions: the flow rate was 1.5mL/min, the column temperature was 35 ℃ and the detection wavelength was 268nm, and the other steps, conditions and the amounts of reagents were the same as in example 1.
Example 7:
a high performance liquid phase detection method of chlorohydrin imine in water.
The procedure, conditions and amounts of reagents were the same as those in example 1 except that the detection wavelength was changed to 260nm under the HPLC analysis conditions.
Examples 8 to 14:
the high performance liquid detection method of chlorohydrin imine in n-octanol comprises the following steps:
the procedures, chromatographic conditions and amounts of reagents used were the same as in examples 1 to 6, respectively, except that the solvent used in step (2) was different.
In examples 7 to 12, the test solution in the step (2) was prepared by the steps of: and (3) sucking 1.00mL of standard sample stock solution with the concentration of 10.0mg/L in the step (1) in the example 1 into a 100mL volumetric flask, metering the volume to the scale with n-octanol, and uniformly mixing to obtain a test solution.
Experimental example:
to illustrate the advantageous effects of the present invention, the present invention provides the following test examples:
1. high performance liquid chromatography analysis condition screening test
1.1 screening test for different sample injection volumes
Selecting 25-35 mu L of sample injection volume for screening test, and carrying out other chromatographic conditions as follows:
and (3) chromatographic column: ZORBAXSB-C18;
flow rate: 1.0mL/min;
mobile phase: a is 0.1% phosphoric acid aqueous solution, B is acetonitrile; a: B =30 (v/v);
column temperature: 30 ℃;
detection wavelength: 254nm.
And (3) test results: under the chromatographic conditions, 25 muL, 28 muL, 30 muL, 32 muL and 35 muL of the test solution in the embodiment 1 are respectively absorbed for determination, the sample injection volume can reach the effect of detecting the chlorhydrin imine within the range of 25 to 35 muL, and the peak separation degree can reach the detection requirement and has good reproducibility. The peak shape is preferable when the injection volume is 30. Mu.L, and therefore, 30. Mu.L is preferable.
1.2 different flow Rate screening test
The flow rate of 0.8-1.5 mL/min is selected for the screening test, and other chromatographic conditions are as follows:
and (3) chromatographic column: ZORBAXSB-C18;
sample introduction volume: 30 mu L of the solution;
mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; a: B =30 (v/v);
column temperature: 30 ℃;
detection wavelength: 254nm.
And (3) test results: under the chromatographic conditions, the test solution in the example 1 is respectively measured by flow rates of 0.8mL/min, 1.0mL/min, 1.2mL/min and 1.5mL/min, the flow rate can reach the effect of detecting the chlorhydrin imine within the range of 0.8-1.5 mL/min, and the peak separation degree can reach the detection requirement and has good reproducibility. The target peak-out time is shortest at a flow rate of 1.0mL/min, and therefore, a flow rate of 1.0mL/min is preferred.
1.3 screening test at different column temperatures
The column temperature of 26-35 ℃ is selected for the screening test, and other chromatographic conditions are as follows:
a chromatographic column: ZORBAXSB-C18;
sample injection volume: 30 mu L of the solution;
flow rate: 1.0mL/min;
mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; a: B =30 (v/v);
detection wavelength: 254nm.
And (3) test results: under the chromatographic conditions, the column temperatures of 26 ℃, 28 ℃, 30 ℃, 32 ℃ and 35 ℃ are respectively set, and the test solution in the embodiment 1 is measured, wherein the column temperature can reach the effect of detecting the chlorhydrine imine within the range of 26-35 ℃, and the peak separation degree can reach the detection requirement. When the column temperature is 30 ℃, the time for peak emergence is the shortest, and therefore, the column temperature is preferably 30 ℃.
1.4 screening assays for different detection wavelengths
Selecting a detection wavelength of 250-260 nm for a screening test, and carrying out other chromatographic conditions as follows:
and (3) chromatographic column: ZORBAXSB-C18;
sample injection volume: 30 mu L of the solution;
flow rate: 1.0mL/min;
mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; a: B =30 (v/v);
column temperature: at 30 ℃.
And (3) test results: under the chromatographic conditions, the test solution in the embodiment 1 is measured by respectively selecting detection wavelengths of 250nm, 252nm, 254nm, 256nm, 258nm and 260nm, the effect of detecting the chlorohydrin imine can be achieved within the range of 250-260 nm, and the peak separation degree can meet the detection requirement. The separation effect and the peak shape are optimum when the detection wavelength is 254nm, and therefore, the detection wavelength is preferably 254nm.
2. Methodology validation test
2.1 specificity
The HPLC analysis method established by the invention is used for measuring blank samples of solvents acetonitrile, water and n-octanol, and spectrograms of the blank samples of the acetonitrile, the water and the n-octanol and a sample to be tested are compared, and the result is shown in figures 2-5, the chlorhydrin imine has a peak at 4.3min, and the blank sample has no interference peak at the time point, which shows that the method has good specificity to the chlorhydrin imine.
2.2 detection and quantitation limits
Analyzing a standard working solution spectrum with the concentration of 0.05mg/L, wherein the signal-to-noise ratio (S/N) =42.03 of a target peak at the concentration, so that the LOD of the method can be considered to be 0.05mg/L; after analyzing the standard working solution pattern at a concentration of 0.10mg/L, the signal-to-noise ratio (S/N) =114.03 at that concentration, and therefore, 0.10mg/L can be used as the LOQ of the present analysis method.
2.3 precision
The same standard working solution with the concentration of 0.40mg/L is addedPerforming continuous sample injection for 6 times, and determining the precision of the analysis method, its RSD R.T. 0.04%, RSD Area Is 0.15%. The result shows that the analysis precision of the same sample can meet the requirement, and the precision test result is shown in table 2.
Table 2: results of precision test
2.4 recovery test
2.4.1 recovery in Water test
Sucking 1.00mL of standard stock solution with the concentration of 10.0mg/L into a 100mL volumetric flask, fixing the volume to the scale with ultrapure water, and uniformly mixing to obtain the low-concentration recovery rate test solution with the concentration of the chlorhydrin imine of 0.10mg/L. The above operations were repeated to prepare 5 parts of a low concentration recovery test solution having a concentration of 0.10mg/L.
And (3) sucking 1.00mL of standard mother liquor with the concentration of 1002.5mg/L into a 100mL volumetric flask, metering to a scale with ultrapure water, and uniformly mixing to obtain a high-concentration recovery rate test solution with the chlorhydrin imine concentration of 10.0mg/L. By repeating the above operation, 5 parts of a high concentration recovery test solution having a concentration of 10.0mg/L was prepared and diluted 20 times with acetonitrile before the measurement.
And simultaneously preparing an ultrapure water blank sample.
The low concentration recovery rate test solution, the high concentration recovery rate test solution and the ultrapure water blank sample are respectively sampled and then tested according to the high performance liquid chromatography analysis conditions of the invention, and the recovery rate is calculated, and the results are shown in table 3.
Table 3: test results of recovery in Water
2.4.2 test of recovery in n-octanol
Sucking 1.00mL of standard stock solution with the concentration of 10.0mg/L into a 100mL volumetric flask, fixing the volume to the scale with n-octanol, and uniformly mixing to obtain the low-concentration recovery rate test solution with the concentration of the chlorohydrin imine of 0.10mg/L. The above operations were repeated to prepare 5 parts of a low concentration recovery test solution having a concentration of 0.10mg/L.
And (3) sucking 1.00mL of standard mother liquor with the concentration of 1002.5mg/L into a 100mL volumetric flask, fixing the volume to a scale by using n-octanol, and uniformly mixing to obtain a high-concentration recovery rate test solution with the concentration of 10.0mg/L of chlorohydrin imine. By repeating the above operation, 5 parts of a high concentration recovery test solution having a concentration of 10.0mg/L was prepared and diluted 20 times with acetonitrile before the measurement.
Simultaneously, a blank sample of n-octanol was prepared.
The low-concentration recovery rate test solution, the high-concentration recovery rate test solution and the n-octanol blank sample are respectively sampled and then tested according to the high performance liquid chromatography analysis conditions of the invention, the recovery rate is calculated, and the results are shown in table 4.
Table 4: recovery in n-octanol
Although the present invention has been described in detail by way of preferred embodiments and with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications or alterations of the embodiments of the present invention may be made by those skilled in the art without departing from the spirit and scope of the invention, and such modifications or alterations are intended to be within the scope of the present invention. Any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present disclosure, and all such changes or substitutions are included in the scope of the present disclosure. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The method for detecting the high performance liquid phase and the content of the chlorohydrin imine is characterized by comprising the following detection steps:
(1) Preparation of standard working solution: weighing a proper amount of chlorhydrin imine standard substance, adding a solvent to dissolve and dilute the chlorhydrin imine standard substance to prepare a series of standard working solutions;
(2) Preparing a test solution: weighing a sample to be tested with a proper amount of chlorhydrin imine, adding a solvent to dissolve and dilute the sample to be tested to prepare a test solution;
(3) Measurement and calculation: injecting the blank solvent, the sample solution of chlorhydrin imine and the standard sample solution of chlorhydrin imine into a high performance liquid chromatograph for analysis, recording a chromatogram, and calculating the content of chlorhydrin imine in the sample solution according to an external standard method.
2. The method according to claim 1, wherein the solvent is acetonitrile, ultrapure water or n-octanol.
3. The method for detecting and measuring the content of chlorohydrin imine according to claim 1, wherein the high performance liquid chromatography comprises a ZORBAX SB-C18 column and a PAD detector, and the analysis conditions of the high performance liquid chromatography are as follows:
sample introduction volume: 25-35 μ L;
flow rate: 0.8-1.5 mL/min;
mobile phase: a is 0.1% phosphoric acid water solution, B is acetonitrile; a: B =30 (v/v);
column temperature: 26 to 35 ℃;
detection wavelength: 250-260 nm.
4. The method for detecting the HPLC and determining the content of chlorohydrin imine according to claim 3, wherein the sample injection volume is 28-32 μ L, the flow rate is 1.0-1.2 mL/min, and the column temperature is 28-32 ℃.
5. The method for detecting and measuring the content of chlorohydrin imine according to claim 4, wherein the sample injection volume is 30 μ L, the flow rate is 1.0mL/min, and the column temperature is 30 ℃.
6. The method according to claim 3, wherein the detection wavelength is 254nm.
7. The method for detecting and measuring the content of chlorohydrin imine according to claim 1, wherein the concentration of the sample solution is 0.10-10.0 mg/L.
8. The method for detecting and measuring the content of chlorohydrin imine according to claim 1, wherein the concentration of the standard working solution is 0.05-10.00 mg/L.
9. The method for detecting and measuring the content of chlorohydrin imine in high performance liquid according to claim 1, wherein the content measurement comprises the following steps:
(1) preparation of standard working solutions: accurately weighing 0.10025g of chlorohydrin imine standard substance in a 100mL volumetric flask, dissolving the chlorohydrin imine standard substance with acetonitrile to a constant volume to a scale, shaking up to obtain a standard mother solution with the concentration of 1002.5mg/L, putting 1.00mL of the standard mother solution in the 100mL volumetric flask, dissolving the standard mother solution with acetonitrile to a constant volume to a scale, shaking up to obtain a standard stock solution with the concentration of 10.00mg/L, and absorbing a proper amount of the standard stock solution to dilute the standard stock solution with acetonitrile to prepare a series of standard working solutions with the concentration of chlorohydrin imine of 0.05, 0.10, 0.20, 0.40, 0.60, 0.80 and 1.00 mg/L;
(2) preparing a test solution: weighing 0.01-1.00 mg of chlorhydrin imine sample to be detected in a 100mL volumetric flask, diluting the volume to a scale with ultrapure water or n-octanol, and mixing uniformly to obtain chlorhydrin imine sample solution;
(3) drawing a standard curve: sucking 25-35 mu L of the series of standard working solutions in the step (1) for HPLC determination, drawing a standard curve by taking the concentration of the series of standard working solutions as a horizontal ordinate and the peak area of the chlorohydrin imine as a vertical coordinate, and solving a regression equation and a correlation coefficient;
(4) sample determination and content calculation: and (3) sucking 25-35 mu L of the sample solution in the step (2) for HPLC determination to obtain the peak area of the chlorhydrin imine in the sample, and substituting the peak area into the linear regression equation in the step (3) for calculation to obtain the concentration of the chlorhydrin imine in the sample.
10. The method for HPLC detection and content determination of chlorohydrin imine according to claim 9, wherein the linear regression equation of chlorohydrin imine is Y =128852X +787.02, and the linear correlation coefficient R is 2 ＝0.9998。
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