CN112326837A - Method for determining content of dichlorides in sulfentrazone by gas chromatography - Google Patents
Method for determining content of dichlorides in sulfentrazone by gas chromatography Download PDFInfo
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- CN112326837A CN112326837A CN202011230203.1A CN202011230203A CN112326837A CN 112326837 A CN112326837 A CN 112326837A CN 202011230203 A CN202011230203 A CN 202011230203A CN 112326837 A CN112326837 A CN 112326837A
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- G—PHYSICS
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- 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
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- 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
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- 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
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- 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
- G01N2030/042—Standards
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Abstract
The invention relates to a method for determining the content of dichlorides in sulfentrazone by using a gas chromatography, which comprises the following steps: 1) preparing a standard solution and a sample solution, A, weighing a dichloride reference substance into a weighing bottle, adding an internal standard solution for dissolving, and shaking up to obtain the standard solution; B. sampling sulfentrazone, weighing the sample into a weighing bottle, adding an equivalent internal standard solution for dissolving, and shaking up to obtain a sample solution; the internal standard solution is a DMF solution of nonadecane; the purity of the dichloride reference substance is Purtiy; 2) performing gas chromatographic analysis, namely performing chromatographic analysis on the sample solution and the standard solution respectively through a gas chromatograph to respectively obtain chromatograms of the sample solution and the standard solution; and is derived from the chromatogram; 3) computing
Description
Technical Field
The invention relates to the field of medicines, and particularly relates to a method for determining the content of dichlorine in sulfentrazone by using a gas chromatography.
Background
Sulfentrazone is a low-toxicity and low-residue herbicide for crops, and has little harm to farmlands, water bodies and crops. The sulfentrazone dichloride is a key intermediate for synthesizing sulfentrazone technical, the content and the quality of the sulfentrazone dichloride directly influence the quality of a final product, and the content result has great significance for accurately controlling the feeding amount.
Disclosure of Invention
The invention provides a method for determining the content of dichlorine in sulfentrazone by using a gas chromatography.
The technical scheme of the invention is as follows:
a method for determining the content of dichlorides in sulfentrazone by gas chromatography, which comprises the following steps:
1) preparing standard solution and sample solution
A. Weighing the dichlorine reference substance into a weighing bottle, adding the internal standard solution for dissolving, and shaking up to obtain the standard solution.
B. Sampling sulfentrazone, weighing the sample into a weighing bottle, adding an equal amount of internal standard solution for dissolving, and shaking up to obtain a sample solution.
The internal standard solution is a DMF solution of nonadecane; the purity of the dichloride control was Purtiy.
2) Gas chromatography analysis
Respectively carrying out chromatographic analysis on the sample solution and the standard solution through a gas chromatograph to respectively obtain chromatograms of the sample solution and the standard solution; and is derived from the chromatogram.
In the standard solution: concentration of internal standard substance cInternal standardPeak area of internal standard substance is aInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit。
In the sample solution: concentration of internal standard substance is CInternal standardThe peak area of the internal standard substance is AInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit。
3) Computing
The calculation formula is as follows:
RF is a correction factor, and Wt is the content of dichlorides in the sulfentrazone.
A method for determining the content of dichlorides in sulfentrazone by gas chromatography, which comprises the following steps:
1) preparing standard solution and sample solution
A. And weighing the dichlorine reference substance into a weighing bottle, adding the internal standard solution for dissolving, and shaking up to obtain the standard solution 1.
B. And weighing the dichlorine reference substance into a weighing bottle, adding an equivalent internal standard solution for dissolving, and shaking up to obtain a standard solution 2.
C. Weighing the dichlorine reference substance into a weighing bottle, adding an equivalent internal standard solution for dissolving, and shaking up to obtain a standard solution 3.
D. Sampling sulfentrazone, weighing the sample into a weighing bottle, adding an equal amount of internal standard solution for dissolving, and shaking up to obtain a sample solution.
The internal standard solution is a DMF solution of nonadecane of 2.0g/1000ml and is used as an internal standard solution; the purity of the dichloride reference substance is Purtiy; the amount of the control of dichloride in all standard solutions 1, 2, 3 was linear.
2) Respectively carrying out gas chromatography analysis on all the standard solutions through a gas chromatograph, and respectively obtaining chromatograms of the sample solution and the standard solutions 1, 2 and 3; and is derived from the chromatogram.
Standard solution 1: concentration of internal standard substance cInternal standard 1Peak area of internal standard substance is aInternal standard 1The concentration of the dichlorine compound is CStandard 1The peak area of the dichloride is AStandard 1。
Standard solution 2: concentration of internal standard substance cInternal standard 2Peak area of internal standard substance is aInternal standard 2The concentration of the dichlorine compound is CStandard 2The peak area of the dichloride is AStandard 2。
Standard solution 3: concentration of internal standard substance cInternal standard 3Peak area of internal standard substance is aInternal standard 3The concentration of the dichlorine compound is CStandard 3The peak area of the dichloride is AStandard 3。
In the sample solution: concentration of internal standard substance is CInternal standardThe peak area of the internal standard substance is AInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit。
3) Computing
The calculation formula is as follows:
RF1、RF2、RF3as a correction factor, Wt is the content of dichlorine in the sulfentrazone.
The parameters of the gas chromatograph are set as follows,
a chromatographic column: agilent DB-130 m × 0.53mm, 1.5 μm column.
Sample inlet temperature: at 250 ℃ to obtain a mixture.
Column temperature: the initial temperature is 150 ℃, the temperature is kept for 3min, and then the temperature is increased to 270 ℃ at the heating rate of 12 ℃/min, and the temperature is kept for 4 min.
Detector temperature: at 300 ℃.
Sample introduction amount: 2.0. mu.l.
The split ratio is as follows: 10: 1.
flow rate of carrier gas: 10 ml/min.
Hydrogen flow rate: 35 ml/min.
Air flow rate: 350 ml/min.
Tail-blow flow rate: 25 ml/min.
Operating time: and (5) 17 min.
Preferably, the chromatograph is an Agilent 7890 gas chromatograph with an autosampler.
In carrying out the inventive concept, we have made relevant experiments:
1) the specificity of the test is tested,
the specificity of the method is examined by feeding a test solution containing all potential impurities as a specific solution. The relative retention time and the degree of separation of each potential impurity under the measurement conditions are determined by a specificity test, so that the concerned impurity can be detected, and the blank solution is free from interference at the retention time of the sulfentrazone dichloride.
As a result: in the blank solution, no interference peak exists at the retention time of the dichlorine peak, and no interference exists at the hexadecane position of the internal standard substance; all peaks are separated from the main peak, and the separation degree is more than or equal to 1.5.
The peak time of the dichlorine is 6.6 min; the peak time of the internal standard substance is 3.2 min; the degree of separation of the dichloride from the adjacent peak was 12.1; the separation of the internal standard from the adjacent peaks was 9.8.
2) And (3) accuracy test:
the accuracy of the method was achieved by examining samples at different concentrations. Concentrations considered included 50%, 80%, 100%, 120%, 150% of the working standard concentration. Each concentration is repeated for 3 times, the recovery rate reaches more than 98.5 percent and meets 100 +/-10 percent; the relative standard deviation reaches below 0.4 percent, and is less than or equal to 5 percent.
The accuracy is calculated from the measured/added values x 100%.
3) And (3) repeatability test:
precision testing was performed by both method repeatability and intermediate precision. The method has the repeatability that the content of the dichloride in each solution is calculated and the relative standard deviation of the result is considered by repeatedly preparing the same batch of test articles for 6 times and injecting 2 needles each time, and the RSD is 0.3 percent and is not more than 10 percent; the intermediate precision is repeatedly verified by different analysts on different working days and by different instruments, and the RSD is 0.7 percent and is not more than 10 percent; and the relative deviation of the repeatability of the method and the intermediate precision result is not more than 10 percent, thereby meeting the requirements.
4) Linear and Range testing
The linearity of the method is achieved by examining the linearity of at least 5 different concentration solutions. The measured peak areas are plotted against the concentration with good linearity and the range of the measurement is determined at the same time.
By testing 5 different concentrations of l-carnitine solutions, the linear equation of concentration versus peak area Y =232854.8x-324.6, R2=0.9996, Y intercept bias of-0.28%, linear range from 50% (1 mg/g) working concentration to 150% (3 mg/g) working concentration was obtained.
5) Stability test of solution
A proprietary solution was prepared for solution stability testing (at least 48 hours). The samples were injected at 0, 3, 6, 12, 24 and 48 hours for detection. The absolute deviation of the content of the dichlorides in the solution in X hours and 0 hour is not more than 0.1 percent, and the solution has good stability in 48 hours. The sample solution needs to be kept sealed to prevent the solution from volatilizing.
6) Durability test
The tolerance of the test method is examined by changing parameters such as carrier gas flow rate, initial column temperature, column temperature rise program and the like. Only one of the parameters was changed for each test, with a range of + -10% for the parameter change, and the results were compared to those measured without changing the parameter. The deviation of the retention time of the dichloride is not more than 15%, the tailing factors of the dichloride are not more than 1.5, the separation degree is not less than 1.5, and the requirements are met.
The invention has the advantages of reasonable design, ingenious conception and simple operation, can quickly and accurately measure the content of the dichlorine in the sulfentrazone, and can ensure good linear range, good stability, and better accuracy and precision, thereby effectively controlling the quality of finished products and ensuring the safety and reliability of production.
Detailed Description
A method for determining the content of dichlorides in sulfentrazone by gas chromatography, which comprises the following steps:
1) preparing standard solution and sample solution
A. Weighing 80mg of the dichlorine reference substance into a weighing bottle, adding 50g of the internal standard solution for dissolving, and shaking up to obtain the standard solution 1.
B. Weighing 100mg of the dichlorine reference substance into a weighing bottle, adding 50g of the internal standard solution for dissolving, and shaking up to obtain a standard solution 2.
C. And weighing 120mg of the dichlorine reference substance into a weighing bottle, adding 50g of the internal standard solution for dissolving, and shaking up to obtain a standard solution 3.
D. Sampling sulfentrazone, weighing 100mg of the sample into a weighing bottle, adding 50g of internal standard solution for dissolving, and shaking up to obtain a sample solution.
The internal standard solution is 2.0g/1000ml DMF solution of nonadecane; the purity of the dichloride reference substance is Purtiy; the amount of the control of dichloride in all standard solutions 1, 2, 3 was linear.
2) Respectively carrying out gas chromatography analysis on all the standard solutions through a gas chromatograph, and respectively obtaining chromatograms of the sample solution and the standard solutions 1, 2 and 3; and is derived from the chromatogram.
Standard solution 1: concentration of internal standard substance cInternal standard 1Peak area of internal standard substance is aInternal standard 1The concentration of the dichlorine compound is CStandard 1The peak area of the dichloride is AStandard 1。
Standard solution 2: concentration of internal standard substance cInternal standard 2Peak area of internal standard substance is aInternal standard 2The concentration of the dichlorine compound is CStandard 2The peak area of the dichloride is AStandard 2。
Standard solution 3: concentration of internal standard substance cInternal standard 3Peak area of internal standard substance is aInternal standard 3The concentration of the dichlorine compound is CStandard 3The peak area of the dichloride is AStandard 3。
In the sample solution: concentration of internal standard substance is CInternal standardThe peak area of the internal standard substance is AInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit。
3) Computing
The calculation formula is as follows:
RF1、RF2、RF3as a correction factor, Wt is the content of dichlorine in the sulfentrazone.
Because of the limited character expression, there exist practically unlimited specific structures, and it will be apparent to those skilled in the art that a number of improvements, decorations, or changes may be made without departing from the principles of the present invention, or the above technical features may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (3)
1. A method for determining the content of dichlorides in sulfentrazone by using a gas chromatography method is characterized by comprising the following steps:
1) preparing standard solution and sample solution
A. Weighing a dichlorine reference substance into a weighing bottle, adding an internal standard solution for dissolving, and shaking up to obtain a standard solution;
B. sampling sulfentrazone, weighing the sample into a weighing bottle, adding an equivalent internal standard solution for dissolving, and shaking up to obtain a sample solution;
the internal standard solution is a DMF solution of nonadecane; the purity of the dichloride reference substance is Purtiy;
2) gas chromatography analysis
Respectively carrying out chromatographic analysis on the sample solution and the standard solution through a gas chromatograph to respectively obtain chromatograms of the sample solution and the standard solution; and is obtained by the chromatogram map, and the chromatogram map is obtained,
in the standard solution: concentration of internal standard substance cInternal standardPeak area of internal standard substance is aInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit；
In the sample solution: concentration of internal standard substance is CInternal standardThe peak area of the internal standard substance is AInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit；
3) Computing
The calculation formula is as follows:
RF is a correction factor, and Wt is the content of dichlorides in the sulfentrazone.
2. A method for determining the content of dichlorides in sulfentrazone by using a gas chromatography method is characterized by comprising the following steps:
1) preparing standard solution and sample solution
A. Weighing a dichloride reference substance into a weighing bottle, adding an internal standard solution for dissolving, and shaking up to obtain a standard solution 1;
B. weighing a dichloride reference substance into a weighing bottle, adding an internal standard solution for dissolving, and shaking up to obtain a standard solution 2;
C. weighing a dichloride reference substance into a weighing bottle, adding an internal standard solution for dissolving, and shaking up to obtain a standard solution 3;
D. sampling sulfentrazone, weighing the sample into a weighing bottle, adding an equivalent internal standard solution for dissolving, and shaking up to obtain a sample solution;
the internal standard solution is a DMF solution of nonadecane of 2.0g/1000ml and is used as an internal standard solution; the purity of the dichloride reference substance is Purtiy; the amount of the control dichlorine in all standard solutions 1, 2, 3 was linear
2) Respectively carrying out gas chromatography analysis on all the standard solutions through a gas chromatograph, and respectively obtaining chromatograms of the sample solution and the standard solutions 1, 2 and 3; and is obtained by the chromatogram map, and the chromatogram map is obtained,
standard solution 1: concentration of internal standard substance cInternal standard 1Peak area of internal standard substance is aInternal standard 1The concentration of the dichlorine compound is CStandard 1The peak area of the dichloride is AStandard 1；
Standard solution 2: concentration of internal standard substance cInternal standard 2Peak area of internal standard substance is aInternal standard 2The concentration of the dichlorine compound is CStandard 2The peak area of the dichloride is AStandard 2；
Standard solution 3: concentration of internal standard substance cInternal standard 3Peak area of internal standard substance is aInternal standard 3The concentration of the dichlorine compound is CStandard 3The peak area of the dichloride is AStandard 3；
In the sample solution: concentration of internal standard substance is CInternal standardThe peak area of the internal standard substance is AInternal standardThe concentration of the dichlorine compound is CStandard of meritThe peak area of the dichloride is AStandard of merit；
3) Computing
The calculation formula is as follows:
RF1、RF2、RF3as a correction factor, Wt is the content of dichlorine in the sulfentrazone.
3. The method for measuring the content of the dichloride in the sulfentrazone by using the gas chromatography as claimed in claim 1 or 2, wherein the parameters of the gas chromatograph are set as follows,
a chromatographic column: agilent DB-130 m × 0.53mm, 1.5 μm chromatography column;
sample inlet temperature: 250 ℃;
column temperature: the initial temperature is 150 ℃, the temperature is kept for 3min, the temperature is raised to 270 ℃ at the heating rate of 12 ℃/min, and the temperature is kept for 4 min;
detector temperature: 300 ℃;
sample introduction amount: 2.0 μ l;
the split ratio is as follows: 10: 1;
flow rate of carrier gas: 10 ml/min;
hydrogen flow rate: 35 ml/min;
air flow rate: 350 ml/min;
tail-blow flow rate: 25 ml/min;
operating time: and (5) 17 min.
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| CN202011230203.1A CN112326837A (en) | 2020-11-06 | 2020-11-06 | Method for determining content of dichlorides in sulfentrazone by gas chromatography |
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| CN202011230203.1A CN112326837A (en) | 2020-11-06 | 2020-11-06 | Method for determining content of dichlorides in sulfentrazone by gas chromatography |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951627A (en) * | 2014-05-06 | 2014-07-30 | 泸州东方农化有限公司 | Method for synthesizing sulfentrazone midbody and sulfentrazone |
| CN109232450A (en) * | 2018-10-25 | 2019-01-18 | 山东润博生物科技有限公司 | A kind of synthetic method of sulfentrazone |
-
2020
- 2020-11-06 CN CN202011230203.1A patent/CN112326837A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951627A (en) * | 2014-05-06 | 2014-07-30 | 泸州东方农化有限公司 | Method for synthesizing sulfentrazone midbody and sulfentrazone |
| CN109232450A (en) * | 2018-10-25 | 2019-01-18 | 山东润博生物科技有限公司 | A kind of synthetic method of sulfentrazone |
Non-Patent Citations (2)
| Title |
|---|
| 张元元 等: "除草剂甲磺草胺的合成", 《农药》 * |
| 汪爱春 等: "甲磺草胺及其关键中间体的合成方法综述", 《精细化工中间体》 * |
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Application publication date: 20210205 |