CN116087376A - Quantitative analysis method for ethylenediamine sulfate - Google Patents

Abstract

The invention provides a quantitative analysis method of ethylenediamine sulfate, which comprises the following steps: the sample is detected by a liquid chromatography-ultraviolet detector (HPLC-UV), p-benzenesulfonyl chloride is used as a derivative, quantitative analysis is carried out on a chromatographic column Nucleosil C18, and the analysis result is calculated. The method is simple, quick and high in accuracy.

Description

Quantitative analysis method for ethylenediamine sulfate

Technical Field

The invention relates to a quantitative analysis method of ethylenediamine sulfate, belonging to the technical field of analytical chemistry.

Background

Ethylenediamine sulfate salt of the formula

The relative molecular weight is 158.18, and the catalyst is easy to dissolve in water, methanol and acetonitrile. In the organic synthesis, the imidazole products are synthesized by the ethylenediamine sulfate and the nitro compounds, and the application are wider. At present, in the production process of ethylenediamine sulfate, due to the existence of impurities such as ammonia and the like, an acid-base titration method is used, so that the error is larger, and the production is not facilitated.

Disclosure of Invention

The invention aims to solve the problems in the existing ethylenediamine sulfate production process and provides a quantitative analysis method of ethylenediamine sulfate with small error.

The technical solution of the invention is as follows: a method for quantitatively analyzing ethylenediamine sulfate uses p-benzenesulfonyl chloride as a derivative, separates and detects a sample by a liquid chromatograph-ultraviolet detector, and quantitatively analyzes the sample by a chromatographic column; the method specifically comprises the following steps:

1) Preparation of derivative solution: weighing analytical pure p-benzenesulfonyl chloride, dissolving in a container, and fixing the volume with methanol; wherein the adding amount of the p-benzenesulfonyl chloride is 2.5g;

2) Standard solution preparation: weighing ethylenediamine sulfate standard sample in a container, transferring the derivative solution prepared in the step 1), and shaking uniformly; wherein the adding amount of the ethylenediamine sulfate is 0.1g, the adding volume of the derivative solution is 1 ml-3 ml,

3) Sample solution preparation: weighing the sample in a container, transferring the derivative solution prepared in the step 1), and shaking uniformly; wherein the addition amount of the sample is 1.0g, the addition volume of the derivative solution is 1 ml-3 ml, and the same as that of the step 2);

4) Sample injection analysis: continuously injecting two needles of standard solution into a liquid chromatograph, injecting the standard solution and the sample solution into the liquid chromatograph after the peak area error of the liquid chromatogram of the two needles of standard solution is less than 1%, measuring by the liquid chromatograph to form a liquid chromatogram, and recording peak area values respectively generated by the standard solution and the sample solution;

5) And calculating the ethylenediamine content according to the peak area value.

Further, the liquid chromatograph in the step 4) is a liquid chromatograph with a UV detector, and the measurement conditions are as follows: mobile phase: acetonitrile and water; wavelength: 224nm; flow rate: 0.8mL/min; sensitivity: 0.05AUFS; sample injection amount: 50ul. The liquid chromatograph adopts a chromatographic column model number of Nucleosil C18, and the specification is 4.0mm (id) multiplied by 250mm; the volume percentages of acetonitrile and water in the mobile phase are respectively 60% and 40%, and 3 drops of phosphoric acid are added dropwise; the injection sequence of the standard solution and the sample solution is as follows: standard solution-sample solution-standard solution.

Further, the calculation formula of the ethylenediamine content in the step 5) is as follows:

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m is in ₁ The weight of the ethylenediamine sulfate standard sample is expressed in g; m is m ₂ Represents the weight of the ethylenediamine sulfate sample in g; a is that ₁ Represents the peak area of ethylenediamine sulfate standard sample; a is that ₂ Represents the peak area of the ethylenediamine sulfuric acid sample; p represents the percent purity of ethylenediamine sulfate standard.

Compared with the prior art, the invention adopts the p-benzenesulfonyl chloride as the derivative reagent, and carries out quantitative analysis on a chromatographic column Nucleosil C18, and the analysis result is calculated. The method is simple, quick and high in accuracy.

Drawings

FIG. 1 is a liquid chromatogram of a sample in example 1 of the present invention.

FIG. 2 is a liquid chromatogram of a sample in example 2 of the present invention.

FIG. 3 is a liquid chromatogram of the sample in example 3 of the present invention.

In the figure, the A-derivatizing agent, the B-derivative.

Detailed Description

The technical scheme of the invention is further described below according to a plurality of embodiments. In the description of the present specification, the contents of each example means that a specific technical feature described in connection therewith is included in at least one embodiment of the present invention. In this specification, a schematic representation of an embodiment does not necessarily refer to the same implementation or example. Furthermore, the particular features described may be combined in any suitable manner in any one or more embodiments or examples.

Example 1

1) Instrument: LC-20A has a UV detector. Chromatographic conditions: chromatographic column: nucleosil C18.0 mm (id). Times.250 mm; mobile phase: acetonitrile + water = 60 +40, add 3 drops of phosphoric acid; wavelength: 224nm; flow rate: 0.8mL/min; sensitivity: 0.05AUFS; sample injection amount: 50uL.

2) The measuring step comprises the following steps:

A. preparation of derivative solution: 2.5g of analytically pure p-benzenesulfonyl chloride was weighed and dissolved in a 500mL volumetric flask and acetonitrile was used to determine the volume.

B. Preparing a standard sample: 0.1g of ethylenediamine sulfate standard sample is weighed, 1mL of the prepared derivative solution is removed from a 25mL triangular flask with a stopper, and the solution is shaken well.

C. Sample preparation: 1.0g (about 50% of ethylenediamine sulfate salt) was weighed out and treated in the same manner as above.

D. Sample injection analysis: and continuously feeding two needles of standard samples, and after the area error is less than 1%, feeding samples according to the sequence of the standard samples, the samples and the standard samples.

E. And (3) calculating results: the calculation formula of the ethylenediamine content is as follows:

m is in ₁ The weight of the ethylenediamine sulfate standard sample is expressed in g; m is m ₂ Represents the weight of the ethylenediamine sulfate sample in g; a is that ₁ Represents the peak area of ethylenediamine sulfate standard sample; a is that ₂ Represents the peak area of the ethylenediamine sulfuric acid sample; p represents the percent purity of ethylenediamine sulfate standard.

The final liquid chromatogram is shown in FIG. 1, and the ethylenediamine sulfate content is 50.05%.

Example 2

1) Instrument: LC-20A has a UV detector. Chromatographic conditions: chromatographic column: nucleosil C18.0 mm (id). Times.250 mm; mobile phase: acetonitrile + water = 60 +40, add 3 drops of phosphoric acid; wavelength: 224nm; flow rate: 0.8mL/min; sensitivity: 0.05AUFS; sample injection amount: 50uL.

2) The measuring step comprises the following steps:

A. preparation of derivative solution: 2.5g of analytically pure p-benzenesulfonyl chloride was weighed and dissolved in a 500mL volumetric flask and acetonitrile was used to determine the volume.

B. Preparing a standard sample: 0.1g of ethylenediamine sulfate standard sample is weighed, 2mL of the prepared derivative solution is removed from a 25mL triangular flask with a stopper, and the solution is shaken well.

C. Sample preparation: 1.0g (about 50% of ethylenediamine sulfate salt) was weighed out and treated in the same manner as above.

D. Sample injection analysis: and continuously feeding two needles of standard samples, and after the area error is less than 1%, feeding samples according to the sequence of the standard samples, the samples and the standard samples.

E. And (3) calculating results: the procedure of example 1, step E, was followed, and the final liquid chromatogram was shown in FIG. 2, to give a calculated ethylenediamine sulfate content of 49.55%.

Example 3

1) Instrument: LC-20A has a UV detector. Chromatographic conditions: chromatographic column: nucleosil C18.0 mm (id). Times.250 mm; mobile phase: acetonitrile + water = 60 +40, add 3 drops of phosphoric acid; wavelength: 224nm; flow rate: 0.8mL/min; sensitivity: 0.05AUFS; sample injection amount: 50uL.

2) The measuring step comprises the following steps:

A. preparation of derivative solution: 2.5g of analytically pure p-benzenesulfonyl chloride was weighed and dissolved in a 500mL volumetric flask and acetonitrile was used to determine the volume.

B. Preparing a standard sample: 0.1g of ethylenediamine sulfate standard sample is weighed, 3mL of the prepared derivative solution is removed from a 25mL triangular flask with a stopper, and the solution is shaken well.

C. Sample preparation: 1.0g (about 50% of ethylenediamine sulfate salt) was weighed out and treated in the same manner as above.

D. Sample injection analysis: and continuously feeding two needles of standard samples, and after the area error is less than 1%, feeding samples according to the sequence of the standard samples, the samples and the standard samples.

E. And (3) calculating results: the procedure of example 1, step E, was followed, and the final liquid chromatogram was shown in FIG. 3, to give a calculated ethylenediamine sulfate content of 50.45%.

The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (10)

1. A method for quantitatively analyzing ethylenediamine sulfate comprises the steps of taking p-benzenesulfonyl chloride as a derivative, separating and detecting a sample by a liquid chromatograph-ultraviolet detector, quantitatively analyzing by a chromatographic column, and calculating the content according to a liquid chromatograph; the method is characterized by comprising the following steps of:

1) Preparation of derivative solution: weighing analytical pure p-benzenesulfonyl chloride, dissolving in a container, and fixing the volume with methanol;

2) Standard solution preparation: weighing ethylenediamine sulfate standard sample in a container, transferring the derivative solution prepared in the step 1), and shaking uniformly;

3) Sample solution preparation: weighing the sample in a container, transferring the derivative solution prepared in the step 1), and shaking uniformly;

4) Sample injection analysis: continuously injecting two needles of standard solution into a liquid chromatograph, injecting the standard solution and the sample solution into the liquid chromatograph after the peak area error of the liquid chromatogram of the two needles of standard solution is less than 1%, measuring by the liquid chromatograph to form a liquid chromatogram, and recording peak area values respectively generated by the standard solution and the sample solution;

5) And calculating the ethylenediamine content according to the peak area value.

2. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the addition amount of the p-benzenesulfonyl chloride in the step 1) is 2.5g.

3. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the addition amount of ethylenediamine sulfate in the step 2) was 0.1g.

4. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the sample in step 3) was added in an amount of 1.0g.

5. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the volumes of the derivative solutions added in the step 2) and the step 3) are 1ml to 3ml, and the volumes of the two additions are the same.

6. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the liquid chromatograph in the step 4) is a liquid chromatograph with a UV detector, and the measurement conditions are as follows: mobile phase: acetonitrile and water; wavelength: 224nm; flow rate: 0.8mL/min; sensitivity: 0.05AUFS; sample injection amount: 50ul.

7. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 6, wherein: the liquid chromatograph adopts a chromatographic column model number of Nucleosil C18, and the specification of the chromatographic column model number is 4.0mm (id) multiplied by 250mm.

8. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 6, wherein: the volume percentages of acetonitrile and water in the mobile phase are respectively 60% and 40%, and 3 drops of phosphoric acid are added dropwise.

9. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 1, wherein: the injection sequence of the standard solution and the sample solution in the step 4) is as follows: standard solution-sample solution-standard solution.

10. The method for quantitative analysis of ethylenediamine sulfate salt according to claim 6, wherein: the calculation formula of the ethylenediamine content in the step 5) is as follows:

m is in ₁ The weight of the ethylenediamine sulfate standard sample is expressed in g; m is m ₂ Represents the weight of the ethylenediamine sulfate sample in g; a is that ₁ Represents the peak area of ethylenediamine sulfate standard sample; a is that ₂ Represents the peak area of the ethylenediamine sulfuric acid sample; p represents the percent purity of ethylenediamine sulfate standard.

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