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2025

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Determination of adenine content by fully automated potentiometric titration


1. Introduction

Adenine is a component of nucleic acids and can promote leukocyte proliferation, increasing the number of white blood cells. It is used to prevent and treat leukopenia caused by various reasons, especially leukopenia caused by chemotherapy for tumors, and also for acute granulocytopenia. The content of a drug is one of the main indicators for evaluating a drug. When studying its determination method, the selection of the content determination method should focus on accuracy, stability, and repeatability. The 2020 edition of the Chinese Pharmacopoeia clearly stipulates the content determination method and content range for adenine. This article refers to the fully automated potentiometric titration method in the pharmacopoeia to determine the content of adenine, which has the characteristics of simple operation, accurate results, and good repeatability.


2. Instruments and Reagents

2.1 Instruments

JH-T6 fully automatic potentiometric titrator, non-aqueous pH composite electrode, 15mL burette unit

2.2 Reagents

Perchloric acid titrant (0.1mol/L), glacial acetic acid, acetic anhydride

3. Experimental Methods

3.1 Experimental Procedure

Accurately weigh 0.1g of the sample into a dry titration cup, add 20mL of acetic anhydride and 30mL of glacial acetic acid solution, and stir until completely dissolved.

Set appropriate parameters and titrate with 0.1mol/L perchloric acid titrant. Perform a blank experiment simultaneously.

3.2 Instrument Parameters

Titration mode: Dynamic titration
Electrode equilibration time:

4s

Minimum addition volume:

0.02

Electrode equilibration potential:

1mv

Ending volume:

10mL

Initial addition volume:

5mL

Potential jump amount

200

 

3.3 Calculation Formula:

In the formula:

X -- sample content (%);

V1 -- volume of perchloric acid titrant consumed during sample titration (mL);

V0 -- volume of perchloric acid titrant consumed during blank titration (mL);

m -- sample weight (g);

c -- concentration of perchloric acid titrant (mol/L).

4 Results and Discussion

4.1 Experimental Results


 

 

 

Number

 

Titrate Concentration (mol/L)

 

Sample Volume (g)

 

Blank Volume (mL)

 

Titration Volume (mL)

 

Content (%)

 

Average Value (%)

1

 

 

 

0.10659

0.10125

 

 

 

0.02

7.003

99.32

 

 

 

99.25

2

0.10199

7.049

99.24

3

0.10071

6.958

99.20

 

4.2 Titration Spectrum

4.3 Experimental Conclusions

The RSD of adenine content determined by fully automated potentiometric titration was 0.06%, with good repeatability. The instrument can automatically control the titration process and determine the endpoint, reducing errors caused by visual endpoint determination, and has the characteristics of being fast and accurate.

References

[1] National Pharmacopoeia Commission. Pharmacopoeia of the People's Republic of China [M]. Volume II. Beijing: China Medical Science and Technology Press, 2020.

Keyword:

automated potentiometric titration