Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method

A high-performance liquid chromatography and flubenimidazole technology, which is applied in the field of chemical detection, can solve problems such as large dosage and affect product quality, and achieve the effects of simple operation and accurate and reliable measurement results.

Inactive Publication Date: 2014-08-13
JIANGSU BAOZONG & BAODA PHARMACHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Acetic acid is one of the solvents used in the production of flubendazole, and it is used in a large amount, so the finished product of flubendazole will contain a small amount of residual acetic acid, which will affect the quality of the product as an impurity

Method used

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  • Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method
  • Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method
  • Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method

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Experimental program
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Effect test

Embodiment 1

[0030] Method for determination of residual acetic acid in flubendazole bulk drug by high performance liquid chromatography:

[0031] Instruments and reagents: LC-2010A high performance liquid chromatography (quaternary pump, degassing unit, UV detector, column oven, automatic sampler, system monitor, LCsolution) (Shimadzu Corporation of Japan); (Manufacturer: Jiangsu Baozhong Baoda Pharmaceutical Co., Ltd., methanol (Merck chromatographically pure), other reagents are analytically pure, and water is self-made fresh redistilled water.

[0032] Chromatographic condition selection: Chromatographic column: ZORBAX SB—C 18 (4.6×250mm, 5μm); mobile phase A: buffer-methanol=950:50 (the buffer is 0.7mL phosphoric acid in 1000mL water, adjust the pH to 3.0 with 1mol?L sodium hydroxide), mobile phase B: methanol, Gradient elution; detection wavelength: 210nm; calculation method: external standard method; flow rate: 1.2 mL?min -1 ; Sensitivity: 1.0 AUFS; Injection volume: 20 μL; Column...

Embodiment 2

[0041] The stability test of the inventive method:

[0042] Take the control solution under Example 1, place it at room temperature for 0, 2, 4, 6, 8, and 10 hours respectively, and then inject samples according to the method in the example. The injection volume is 20 μL. After calculation, the peak area of ​​acetic acid is The RSD is 0.39%, which shows that the method has good stability.

Embodiment 3

[0044] Quantitation limit test of the inventive method:

[0045] Weigh 100mg of glacial acetic acid, add water to dissolve and dilute to contain glacial acetic acid 5μg?mL -1 The solution of the sample is injected according to the method of the embodiment, and the sample injection is 2 times, and each injection volume is 20 μ L, and the chromatogram is recorded, referring to Figure 5 , the peak height of acetic acid in the chromatogram is about 8.7 times of the baseline noise (ie S / N=8.7), then the limit of quantitation of this method is 5 μg?mL -1 , converted to 515ppm according to the concentration of flubendazole sample preparation.

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Abstract

The invention discloses a method for measuring residual acetic acid in a flubendazole crude drug by a high performance liquid chromatography method. The method disclosed by the invention specifically comprises the following step: carrying out gradient elution by adopting an HPLC (high performance liquid chromatography) method and a ZORBAXSB-C18 chromatographic column, taking phosphoric acid solution and methanol of 950 to 50 as a mobile phase A, and adopting methanol as a mobile phase B, wherein detection wavelength is 210 nm, flow speed is 1.2mL.min<-1>. The acetic acid has good linearity (r=0.99999, n=6) within a range of 2.5 mu g.mL<-1>-1014.9 mu g.mL<-1>, a recovery rate of 99.2% and precision RSD (Relative Standard Deviation) of 1.1%. The method for measuring residual acetic acid in flubendazole crude drug by the high performance liquid chromatography method is simple and quick to operate, and accurate and reliable in measured result, so that quality of the drug can be effectively controlled. Gradient elution is adopted on selecting the mobile phases, so that trailing or shoulder peak due to overlong sample peak appearance time is avoided. On selection of a dilution solvent of the main drug, the method disclosed by the invention has the advantage that formic acid as a co-solvent in consideration of a fact that the flubendazole crude drug is not easy to dissolve in water and a normal organic solvent, but better in solubility in acid, so that good effect is achieved.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography method for determining residual acetic acid in flubendazole crude drug, belonging to the field of chemical detection. Background technique [0002] Acetic acid is one of the solvents used in the production of flubendazole, and it is used in a relatively large amount. Therefore, the finished product of flubendazole will contain a small amount of residual acetic acid, which will affect the quality of the product as an impurity. Generally, impurities are allowed to exist in the product within the range allowed by safety. Therefore, it is very necessary and urgent to use chemical analysis methods to detect the content of acetic acid in the product. [0003] At present, general chemical analysis methods are mainly divided into gravimetric analysis, titration analysis, chromatographic analysis, and colorimetric analysis. We know that the detection of simple acetic acid is very common. The dete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/34
Inventor 王琳丁海宏黄俊
Owner JIANGSU BAOZONG & BAODA PHARMACHEM
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