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2025

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Determination of adenosine content by fully automated potentiometric titration


I. Introduction

Adenosine is an important intermediate in the synthesis of adenosine triphosphate (ATP), adenine, adenosine acid, and vidarabine, with the molecular formula C10H13N5O4.

It can directly enter the myocardium, undergo phosphorylation to generate adenosine acid, participate in myocardial energy metabolism, and also participate in the dilation of coronary arteries, increasing blood flow. It has physiological effects on the cardiovascular system and many other systems and tissues of the body. This experiment determined whether the adenosine content of a certain manufacturer's product met the standards.

The Shanghai Jiahang JH-T6 fully automatic potentiometric titrator was used to determine the endpoint by setting the potential jump point, and the content was measured.

II. Instruments and Reagents

2.1 Instruments

JH-T6 fully automatic potentiometric titrator, non-aqueous pH composite electrode, analytical balance, etc.

2.2 Reagents

Glacial acetic acid, 0.1 mol/L perchloric acid standard titrant

III. Experimental Methods

3.1 Experimental Procedure:

1) Determination of adenosine content: Accurately weigh 0.2 g of the sample (accurate to 0.0001 g) and place it in a dry titration cup. Add 40 mL of glacial acetic acid, heat gently to dissolve, place it on the potentiometric titration stage, turn on the stirrer to mix the sample completely, insert the composite electrode and titration head,

start the edited method, titrate with perchloric acid (0.100 mol/L) standard solution to the potential jump point, record the volume of standard titrant consumed, and perform a blank test simultaneously.

3.2 Instrument Parameters

The parameter settings for the JH-T6 fully automatic titrator are shown in Table 1:

表 1 滴定仪参数设置

Titration type: dynamic titration Method Name: Perchloric acid determination of adenosine content
Burette volume:

10mL

Sample Measurement Unit:

g

Working electrode: Non-aqueous pH composite electrode Reference Electrode:

无

Stirring speed:

7

Pre-stirring Time:

5s

Electrode equilibration time:

6s

Electrode Equilibrium Potential:

1mv

Titration speed: slow Equilibrium Potential Before Titration:

6mv

Minimum addition volume:

0.03mL

Final Volume:

20mL

Pre-titration addition volume: 0 (can also be set appropriately) Minimum Addition Volume:

0.02mL

Potential jump:

200mV

Pre-Control mV Value:

无

Correlation coefficient:

26.72

Result Unit:

%

Titrant name: perchloric acid Theoretical Concentration: 0.1 (calibrated concentration)

 

IV. Results and Discussion

4.1 Experimental Results

The samples were tested, and the experimental results are shown in Table 2:

Table 2 Adenosine Content Test Results

 
Sample Name Sample Amount/g c(perchloric acid)/mol/L Blank Volume V1/mL Titration Volume V2/mL Content/% Average Content/%

RSD(%)

 

 

adenosine

0.21785

 

 

0.1018

 

 

0.06

8.055

99.826

 

 

99.463

 

 

0.3479

0.20029

7.381

99.425

0.20935

7.690

99.137

 4.2 Titration Spectrum

4.3 Conclusion

The adenosine content tested in this test using perchloric acid titration was 99.463%, which meets the production requirements. Furthermore, using instrumental judgment reduced human error and greatly improved the accuracy of the experiment. Potentiometric titration is a good choice for detecting this type of sample.

V. Precautions

1. The concentration of the perchloric acid titrant is greatly affected by the ambient temperature. It is recommended to standardize the concentration of the perchloric acid titrant before performing the titration experiment.

VI. References

[1] Chinese Pharmacopoeia 2020 Edition, Part II [M].

Keyword:

automated potentiometric titration