CN106053698A - Quantitative analysis method for ethylenediamine sulfate - Google Patents
Quantitative analysis method for ethylenediamine sulfate Download PDFInfo
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- CN106053698A CN106053698A CN201610513806.XA CN201610513806A CN106053698A CN 106053698 A CN106053698 A CN 106053698A CN 201610513806 A CN201610513806 A CN 201610513806A CN 106053698 A CN106053698 A CN 106053698A
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- ethylenediamine sulfate
- ethylenediamine
- standard solution
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention relates to the field of chemicals, and discloses a quantitative analysis method for ethylenediamine sulfate. The quantitative analysis method comprises the following steps by adopting p-benzenesulfonyl chlorid as a color reagent: preparing a derivative solution, preparing a standard solution, preparing a to-be-tested sample solution, injecting the standard solution, sample solution, sample solution and standard solution into a liquid chromatograph sequentially, determining through the liquid chromatograph to form a liquid chromatogram, recording the peak values of the standard solution and the sample solution, and finally calculating the content of the ethylenediamine sulfate in the to-be-tested sample. The method is operated simply and rapidly, the accuracy of results is high, the reproducibility is good, impurity components are thoroughly separated, and the quantitative analysis method has important meaning on the quality analysis of ethylenediamine sulfate.
Description
Technical field
The present invention relates to chemical field, particularly relate to a kind of ethylenediamine sulfate salt quantitative analysis method.
Background technology
Ethylenediamine sulfate salt
Relative molecular mass is 158.18, soluble in water and methanol and acetonitrile.On organic synthesis, ethylenediamine sulfate salt with
Nitro compound synthesis imidazoles product, has wide application purpose.
Ethylenediamine sulfate salt is in process of production at present, because there being the existence of the impurity such as ammonia, surveys with acid base titration methods analyst
Determining the content of ethylenediamine sulfate salt, error is relatively big, is unfavorable for that production is carried out.
Therefore, in order to ensure the accuracy of measurement result, it is ensured that produce efficiently, it would be highly desirable to study new method to analyze survey
Determine the content of ethylenediamine sulfate salt.
Summary of the invention
The technical problem to be solved is, for analyzing the content measuring ethylenediamine sulfate salt in prior art
The problem that error is bigger, the invention provides a kind of simple to operate, quick, analysis measurement method that result precision is high.
In order to solve above-mentioned technical problem, the invention provides a kind of ethylenediamine sulfate salt quantitative analysis method, analysis side
Specifically comprising the following steps that of method
S1, preparation derivative solution: weigh appropriate to benzene sulfonyl chloride in container 1, use dilution in acetonitrile constant volume；
S2, preparing standard solution: weigh moderate amount of sulfuric acid ethylenediamine in container 2, and in described container 2, add appropriate institute
State the derivative solution in S1, shake up；
S3, preparation testing sample solution: weigh moderate amount of sulfuric acid ethylenediamine salt in container 3, and add in described container 3
Derivative solution in appropriate described S1, shakes up；
S4, sample introduction analysis: the standard solution in S2 and the testing sample solution in S3 are injected chromatograph of liquid, passes through liquid
Chromatography measures, and forms liquid chromatogram, the peak area value that record standard solution and sample solution produce respectively, its Plays
The injection order of solution and testing sample solution is standard solution-testing sample solution-standard solution-testing sample solution；
S5, pass through below equation:Calculate containing of testing sample ethylenediamine sulfate salt
Amount；
In formula:
m1Represent the weight of ethylenediamine sulfate standard solution, unit g；
m2Represent the weight of ethylenediamine sulfate salt testing sample solution, unit g；
A1Represent the peak area that ethylenediamine sulfate standard solution produces；
A2Represent the peak area that ethylenediamine sulfate testing sample solution produces；
P represents the purity of ethylenediamine sulfate standard solution, %.
Preferably, the addition to benzene sulfonyl chloride in described S1 is 2.5g, the addition of the ethylenediamine sulfate in described S2
Amount is 0.1g, and the addition of the ethylenediamine sulfate salt in described S3 is 1.0g, and in the container 1 added in described S2, preparation is derivative
The volume of solution is 1ml 3ml, and in the container 1 added in described S3, the volume of the derivative solution of preparation is 1ml 3ml, described
In the container 1 added in S2 with S3, the volume of the derivative solution of preparation is identical.
Preferably, in described S4, liquid chromatographic detection condition is as follows:
Chromatographic column: Nucleosil C18；
Flowing phase: acetonitrile, water and phosphoric acid；
Type of elution: isocratic elution；
Wavelength: 224nm；
Flow velocity: 0.8ml/min；
Sensitivity: 0.05AUFS；
Sample size: 10ul.
Preferably, the chromatograph of liquid in described S4 is LC-20A chromatograph, and the chromatographic detector of described LC-20A is
UV UV-detector.
Preferably, described chromatographic column specification is 4.0mm (id) × 250mm.
Further, described flowing phase acetonitrile, water and phosphoric acid are standby through membrane filtration and ultrasonic degassing.
Preferably, described isocratic condition is as follows: acetonitrile and the percent by volume of water in flowing mutually are respectively 60%
With 40%.
The invention has the beneficial effects as follows: the method for the present invention is simple to operate, quick, result precision is high, favorable reproducibility, miscellaneous
Matter Component seperation is thorough, the quality analysis important in inhibiting to ethylenediamine sulfate salt, beneficially commercial production.
Accompanying drawing explanation
In order to be illustrated more clearly that technical scheme, below will be to required in embodiment or description of the prior art
The accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only some embodiments of the present invention, right
From the point of view of those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain it according to these accompanying drawings
Its accompanying drawing.
Fig. 1 is the liquid chromatogram of embodiments of the invention 1；
Fig. 2 is the liquid chromatogram of embodiments of the invention 2；
Fig. 3 is the liquid chromatogram of embodiments of the invention 3.
Wherein, in figure, reference corresponds to: the peak area that A1-ethylenediamine sulfate standard solution produces, A2-represents sulphuric acid
The peak area that ethylenediamine testing sample solution produces.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, the present invention will be made the most detailed below
Describe.
Embodiment 1
1. instrument: LC-20A chromatograph UV UV-detector.
2. chromatographic condition:
Chromatographic column: Nucleosil C18 chromatographic column 4.0mm (id) × 250mm；
Flowing phase: acetonitrile, water and phosphoric acid, flowing phase acetonitrile, water and phosphoric acid are standby through membrane filtration and ultrasonic degassing；
The percent by volume of type of elution: isocratic elution, acetonitrile and water is respectively 60% and 40%；
Wavelength: 224nm；
Flow velocity: 0.8ml/min；
Sensitivity: 0.05AUFS；
Sample size: 10ul.
3. concrete analysis determination step:
S1, preparation derivative solution: weigh 2.5g to benzene sulfonyl chloride in 50ml volumetric flask, use dilution in acetonitrile constant volume；
S2, preparing standard solution: weigh 0.1g ethylenediamine sulfate and fill in triangular flask in 25ml tool, pipette in 1ml S1 and prepare
Good derivative solution, shakes up；
S3, preparation testing sample solution: weigh 1.0g ethylenediamine sulfate salt and fill in triangular flask in another 25ml tool, pipette
The derivative solution prepared in 1ml S1, shakes up；
S4, sample introduction analysis: the standard solution in S2 and the testing sample solution in S3 are injected chromatograph of liquid, passes through liquid
Chromatography measures, and forms liquid chromatogram, the peak area value that record standard solution and sample solution produce respectively, its Plays
The injection order of solution and testing sample solution is standard solution-testing sample solution-standard solution-testing sample solution；
S5, result calculate:
In formula:
m1Represent the weight of ethylenediamine sulfate standard solution, unit g；
m2Represent the weight of ethylenediamine sulfate salt testing sample solution, unit g；
A1Represent the peak area that ethylenediamine sulfate standard solution produces；
A2Represent the peak area that ethylenediamine sulfate testing sample solution produces；
P represents the purity of ethylenediamine sulfate standard solution, %；
The ethylenediamine sulfate content recorded is 50.05%.
Embodiment 2
1. instrument: LC-20A chromatograph tool UV UV-detector.
2. chromatographic condition:
Chromatographic column: Nucleosil C18 chromatographic column 4.0mm (id) × 250mm；
Flowing phase: acetonitrile, water and phosphoric acid, flowing phase acetonitrile, water and phosphoric acid are standby through membrane filtration and ultrasonic degassing；
The percent by volume of type of elution: isocratic elution, acetonitrile and water is respectively 60% and 40%；
Wavelength: 224nm；
Flow velocity: 0.8ml/min；
Sensitivity: 0.05AUFS；
Sample size: 10ul.
3. concrete analysis determination step:
S1, preparation derivative solution: weigh 2.5g to benzene sulfonyl chloride in 50ml volumetric flask, use dilution in acetonitrile constant volume；
S2, preparing standard solution: weigh 0.1g ethylenediamine sulfate and fill in triangular flask in 25ml tool, pipette in 2ml S1 and prepare
Good derivative solution, shakes up；
S3, preparation testing sample solution: weigh 1.0g ethylenediamine sulfate salt and fill in triangular flask in another 25ml tool, pipette
The derivative solution prepared in 2ml S1, shakes up；
S4, sample introduction analysis: the standard solution in S2 and the testing sample solution in S3 are injected chromatograph of liquid, passes through liquid
Chromatography measures, and forms liquid chromatogram, the peak area value that record standard solution and sample solution produce respectively, its Plays
The injection order of solution and testing sample solution is standard solution-testing sample solution-standard solution-testing sample solution；
S5, result calculate:
In formula:
m1Represent the weight of ethylenediamine sulfate standard solution, unit g；
m2Represent the weight of ethylenediamine sulfate salt testing sample solution, unit g；
A1Represent the peak area that ethylenediamine sulfate standard solution produces；
A2Represent the peak area that ethylenediamine sulfate testing sample solution produces；
P represents the purity of ethylenediamine sulfate standard solution, %；
The ethylenediamine sulfate content recorded is 49.55%.
Embodiment 3
1. instrument: LC-20A chromatograph tool UV UV-detector.
2. chromatographic condition:
Chromatographic column: Nucleosil C18 chromatographic column 4.0mm (id) × 250mm；
Flowing phase: acetonitrile, water and phosphoric acid, flowing phase acetonitrile, water and phosphoric acid are standby through membrane filtration and ultrasonic degassing；
The percent by volume of type of elution: isocratic elution, acetonitrile and water is respectively 60% and 40%；
Wavelength: 224nm；
Flow velocity: 0.8ml/min；
Sensitivity: 0.05AUFS；
Sample size: 10ul.
3. concrete analysis determination step:
S1, preparation derivative solution: weigh 2.5g to benzene sulfonyl chloride in 50ml volumetric flask, use dilution in acetonitrile constant volume；
S2, preparing standard solution: weigh 0.1g ethylenediamine sulfate and fill in triangular flask in 25ml tool, pipette in 3ml S1 and prepare
Good derivative solution, shakes up；
S3, preparation testing sample solution: weigh 1.0g ethylenediamine sulfate salt and fill in triangular flask in another 25ml tool, pipette
The derivative solution prepared in 3ml S1, shakes up；
S4, sample introduction analysis: the standard solution in S2 and the testing sample solution in S3 are injected chromatograph of liquid, passes through liquid
Chromatography measures, and forms liquid chromatogram, the peak area value that record standard solution and sample solution produce respectively, its Plays
The injection order of solution and testing sample solution is standard solution-testing sample solution-standard solution-testing sample solution；
S5, result calculate:
In formula:
m1Represent the weight of ethylenediamine sulfate standard solution, unit g；
m2Represent the weight of ethylenediamine sulfate salt testing sample solution, unit g；
A1Represent the peak area that ethylenediamine sulfate standard solution produces；
A2Represent the peak area that ethylenediamine sulfate testing sample solution produces；
P represents the purity of ethylenediamine sulfate standard solution, %.
The ethylenediamine sulfate content recorded is 50.45%.
The invention has the beneficial effects as follows: the method for the present invention is simple to operate, quick, result precision is high, favorable reproducibility, miscellaneous
Matter Component seperation is thorough, the quality analysis important in inhibiting to ethylenediamine sulfate salt, beneficially commercial production.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (7)
1. an ethylenediamine sulfate salt quantitative analysis method, it is characterised in that comprise the steps of
S1, preparation derivative solution: weigh appropriate to benzene sulfonyl chloride in container 1, use dilution in acetonitrile constant volume；
S2, preparing standard solution: weigh moderate amount of sulfuric acid ethylenediamine in container 2, and in described container 2, add appropriate described S1
In derivative solution, shake up；
S3, preparation testing sample solution: weigh moderate amount of sulfuric acid ethylenediamine salt in container 3, and add appropriate in described container 3
Derivative solution in described S1, shakes up；
S4, sample introduction analysis: the standard solution in S2 and the testing sample solution in S3 are injected chromatograph of liquid, by liquid phase color
Spectrometer measures, and forms liquid chromatogram, the peak area value that record standard solution and sample solution produce respectively, wherein standard solution
Injection order with testing sample solution is standard solution-testing sample solution-standard solution-testing sample solution；
S5, pass through below equation:Calculate the content of testing sample ethylenediamine sulfate salt；
In formula:
m1Represent the weight of ethylenediamine sulfate standard solution, unit g；
m2Represent the weight of ethylenediamine sulfate salt testing sample solution, unit g；
A1Represent the peak area that ethylenediamine sulfate standard solution produces；
A2Represent the peak area that ethylenediamine sulfate testing sample solution produces；
P represents the purity of ethylenediamine sulfate standard solution, %.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 1, it is characterised in that right in described S1
The addition of benzene sulfonyl chloride is 2.5g, and the addition of the ethylenediamine sulfate in described S2 is 0.1g, the sulphuric acid second two in described S3
The addition of amine salt is 1.0g, and in the container 1 added in described S2, the volume of the derivative solution of preparation is 1ml 3ml, described S3
In the container 1 of middle addition, the volume of the derivative solution of preparation is 1ml 3ml, preparation in the container 1 added in described S2 and S3
The volume of derivative solution is identical.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 1, it is characterised in that liquid phase in described S4
Chromatographic test strip part is as follows:
Chromatographic column: Nucleosil C18；
Flowing phase: acetonitrile, water and phosphoric acid；
Type of elution: isocratic elution；
Wavelength: 224nm；
Flow velocity: 0.8ml/min；
Sensitivity: 0.05AUFS；
Sample size: 10ul.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 1, it is characterised in that the liquid in described S4
Chromatography is LC-20A chromatograph, and the chromatographic detector of described LC-20A is UV UV-detector.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 3, it is characterised in that described chromatographic column is advised
Lattice are 4.0mm (id) × 250mm.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 3, it is characterised in that described flowing phase second
Nitrile, water and phosphoric acid are standby through membrane filtration and ultrasonic degassing.
A kind of ethylenediamine sulfate salt quantitative analysis method the most according to claim 3, it is characterised in that described isocratic elution
Condition is as follows: acetonitrile and the percent by volume of water in flowing mutually are respectively 60% and 40%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298092A (en) * | 2018-11-01 | 2019-02-01 | 常州合全药业有限公司 | Detect the HPLC method of sulfonyloxy methyl chlorinity in industrial wastes |
| CN111721847A (en) * | 2019-03-21 | 2020-09-29 | 成都倍特药业股份有限公司 | Method for detecting content of ethylenediamine in medicine by HPLC |
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| US20090216023A1 (en) * | 2004-05-03 | 2009-08-27 | Lanter James C | Novel indole derivatives as selective androgen receptor modulators (sarms) |
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2016
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| JPH0273067A (en) * | 1988-09-09 | 1990-03-13 | Asahi Chem Ind Co Ltd | Novel ethylenediamine derivative and acid addition salt thereof |
| US20090216023A1 (en) * | 2004-05-03 | 2009-08-27 | Lanter James C | Novel indole derivatives as selective androgen receptor modulators (sarms) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298092A (en) * | 2018-11-01 | 2019-02-01 | 常州合全药业有限公司 | Detect the HPLC method of sulfonyloxy methyl chlorinity in industrial wastes |
| CN109298092B (en) * | 2018-11-01 | 2021-07-20 | 常州合全药业有限公司 | HPLC method for detecting content of methylsulfonyl chloride in industrial waste liquid |
| CN111721847A (en) * | 2019-03-21 | 2020-09-29 | 成都倍特药业股份有限公司 | Method for detecting content of ethylenediamine in medicine by HPLC |
| CN111721847B (en) * | 2019-03-21 | 2022-11-01 | 成都倍特药业股份有限公司 | Method for detecting content of ethylenediamine in medicine by HPLC |
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Application publication date: 20161026 |