Method for determining phenylhydrazine and phenylhydrazine derivative in medicine or synthetic intermediate by derivatization HPLC-DAD method

A derivative and derivatization technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as low sensitivity, many interferences, and large baseline noise

Inactive Publication Date: 2019-03-26
CHINA PHARM UNIV
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Problems solved by technology

However, most drugs or synthetic intermediates have strong ultraviolet absorption, and the content of drugs or synthetic intermediates is large. It is necessary to establish a chromatographic condition to separate drugs and impurities. There are many interferences and low sensitivity (big baseline noise), which will interfere Quantitative detection of trace impurities

Method used

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  • Method for determining phenylhydrazine and phenylhydrazine derivative in medicine or synthetic intermediate by derivatization HPLC-DAD method
  • Method for determining phenylhydrazine and phenylhydrazine derivative in medicine or synthetic intermediate by derivatization HPLC-DAD method
  • Method for determining phenylhydrazine and phenylhydrazine derivative in medicine or synthetic intermediate by derivatization HPLC-DAD method

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preparation example Construction

[0042] 1.3. Solution preparation

[0043] 1.3.1 Phenylhydrazine stock solution:

[0044] Take about 10 mg of phenylhydrazine, weigh it accurately, place it in a 10 mL measuring bottle, dilute to the mark with acetonitrile, and shake well. Precisely measure 100 μL of the above solution, place it in a 10 mL measuring bottle, dilute to the mark with acetonitrile, and shake well. The concentration of phenylhydrazine in the stock solution is 10 μg / mL.

[0045] 1.3.2 p-sulfonamidophenylhydrazine stock solution:

[0046] Take about 10 mg of p-sulfonamidophenylhydrazine (CAS No. 4392-54-5), weigh it accurately, place it in a 10 mL measuring bottle, dilute to the mark with acetonitrile, and shake well. Precisely measure 100 μL of the above solution, place it in a 10 mL measuring bottle, dilute to the mark with acetonitrile, and shake well. The concentration of p-sulfonamidophenylhydrazine in the stock solution is 10 μg / mL.

[0047] 1.3.3 Derivatization test solution:

[0048] 2-nit...

Embodiment 1

[0055] The comparison of embodiment 1 derivatization reagent

[0056] Precisely pipette 1mL of 10μg / mL phenylhydrazine stock solution, put it in a 10mL volumetric flask, add 1mL of benzaldehyde derivatization test solution, dilute to the mark with acetonitrile-water (80:20, v / v), shake uniform. After reacting at room temperature for 45 minutes, 20 μL was injected into HPLC-DAD for analysis.

[0057] HPLC-DAD conditions: Shimadzu LC 20AT liquid chromatograph (including online vacuum degasser, binary gradient pump, autosampler, column oven, DAD detector and LC-solution chromatographic workstation); chromatographic column adopts 250mm× 4.6mm, 5μm Diamonsil TM C18 column; injection volume: 20 μL; mobile phase: acetonitrile-0.1% phosphoric acid aqueous solution (70:30, v / v), isocratic elution; flow rate: 1.0mL / min; column temperature: 30°C; detection wavelength: 416nm . Record the spectrum and chromatogram of the product, and use the maximum absorption wavelength and absorptio...

Embodiment 2

[0060] Example 2 Derivatization condition optimization

[0061] In order to ensure the efficiency of the derivatization reaction, the concentration of the derivatization reagent in the system, the reaction time, the reaction temperature and the proportion of the organic phase were investigated. Taking the peak area of ​​the derivative product of phenylhydrazine and 4-nitrobenzaldehyde as an index, the water content of the reaction system (1, 5, 8, 10, 20, 30, 50, 70%, v / v ), 4-nitrobenzaldehyde concentration (0.2,0.5,1.0,2.0,2.5,3.0,4.0,5.0mg / ml), reaction time (15,30,45,60,90,120,180min) and reaction Effect of temperature (25, 40, 60, 80°C) on derivatization reaction efficiency, the results are as follows image 3 Shown; In the experiment, the concentration of phenylhydrazine in the system was 1 μg / mL.

[0062] Depend on image 3 In A, it can be seen that adding a certain volume of water in the reaction system is beneficial to the derivatization reaction, and the peak area...

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Abstract

The invention discloses a method for determining phenylhydrazine and phenylhydrazine derivatives in medicine or synthetic intermediate by a derivatization HPLC-DAD method. The method is characterizedin that a benzaldehyde type derivatization reagent, and the phenylhydrazine and the phenylhydrazine derivative react to generate a product has strong absorption performance in a near visible light-visible light region; derivatization reaction liquid is used as a sample; the reaction product of the phenylhydrazine and the phenylhydrazine derivative is determined in the near visible light-visible light region on the basis of reversed-phase high performance liquid chromatography principle, so that the qualitative or quantitative detection of the phenylhydrazine and the phenylhydrazine derivativeis realized; the absorption wavelength of the derivatization product has obvious redshift, so that the substrate interference of the medicine or synthetic intermediate can be effectively avoided. Inaddition, the methodology validation result shows that the method has high specificity and sensitivity.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, in particular to a method for determining phenylhydrazine and its derivatives in drugs or synthetic intermediates by a derivatization HPLC-DAD method. Background technique [0002] Impurities in drugs are other substances introduced during the production and storage of active pharmaceutical ingredients (Active Pharmaceutical Ingredients, APIs) or preparations [1] . Even if some impurities exist in the drug at a trace level, it will also affect the activity and safety of the drug, and have a serious impact on the risk assessment of the drug. Genotoxic impurities (Genotoxic impurities, GTIs) are a class of compounds that can interact with the genetic material of organisms to produce toxicity. happened [2] . In recent years, with the gradual improvement of genotoxic impurity regulations, the United States Food and Drug Administration (FDA) and the European Medicines Agency (European Me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 刘晶郑枫纳丁·乔尔·俄友罗·诺亚高鸿彬
Owner CHINA PHARM UNIV
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