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Method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV/Vis

A technology of HPLC-UV and nitrobenzaldehyde, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inapplicability to laboratory routine testing and lack of specificity

Inactive Publication Date: 2018-11-16
CHINA PHARM UNIV
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Problems solved by technology

It has also been reported that the use of 3-nitrophenylhydrazine (3-NPH) [23] For the quantitative analysis of fatty aldehydes in human plasma samples, it is determined by mass spectrometry detector, but it is not suitable for routine detection in laboratories
In addition, there is no report on the systematic comparison of nitrophenylhydrazine reagents for the derivatization of aldehydes
[0005] Among various separation and analysis methods, the HPLC-UV / Vis method has become the preferred method for most laboratories because of its simplicity and practicality. However, due to the strong ultraviolet absorption of most drugs and their related substances, the lack of specificity is a problem. The main flaw of the law

Method used

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  • Method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV/Vis
  • Method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV/Vis
  • Method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV/Vis

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Experimental program
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preparation example Construction

[0041] 1.3. Preparation of solution

[0042] 4-Nitrobenzaldehyde stock solution: Take about 10mg of 4-nitrobenzaldehyde, accurately weigh it, place it in a 10mL volumetric flask, dilute to the mark with acetonitrile-water with a volume concentration of 70% acetonitrile, and shake it well. .

[0043] 2-Nitrophenylhydrazine hydrochloride, 3-nitrophenylhydrazine hydrochloride, 4-nitrophenylhydrazine hydrochloride and 2,4-dinitrophenylhydrazine hydrochloride test solution (hereinafter referred to as 2-NPH ·HCl, 3-NPH·HCl, 4-NPH·HCl and 2,4-DNPH·HCl): Take about 100mg of each reagent, accurately weigh it, and place it in a 10mL volumetric flask. Dilute to the mark with 80% acetonitrile. Shake well. Need to be freshly prepared. Among them, 2,4-dinitrophenylhydrazine hydrochloride is first dissolved with an appropriate amount of N,N-dimethylacetamide.

[0044] 1.4. Experimental conditions for derivatization

[0045] Precisely weigh the appropriate amount of medicines, or accurately pipet...

Embodiment 1

[0049] Taking 4-nitrobenzaldehyde as the test substance, it was derivatized with 4 nitrophenylhydrazine derivatizing reagents of the same concentration. See 1.4 for derivatization experimental conditions. Under the same chromatographic conditions, scan each derivatization product with DAD, record the spectrum and chromatogram of the product, and evaluate the quality of the derivatization reagent with the maximum absorption wavelength and absorption intensity of the product.

[0050] figure 1 It shows that except for 3-nitrophenylhydrazine, the maximum absorption wavelengths of the other three derivatization reagents are all above 350nm, which are 426nm (2-nitrophenylhydrazine), 384nm (4-nitrophenylhydrazine) and 356nm ( 2,4-Dinitrophenylhydrazine), which can be attributed to the electron withdrawing ability of the nitro group at the ortho and / or para position on the benzene ring of phenylhydrazine. The maximum absorption wavelength of 3-nitrophenylhydrazine is only 225nm, and th...

Embodiment 2

[0054] In order to ensure that the derivatization reaction proceeds quickly and the reaction is complete, the amount of derivatization reagent in the system, the reaction time, the reaction temperature and the ratio of the organic phase need to be investigated. Taking the peak area of ​​the resulting 4-nitrobenzaldehyde derivatization product as an indicator, a single factor test investigated different concentrations of 3-nitrophenylhydrazine hydrochloride (0.1, 0.2, 0.5, 1.0, 1.5, 2.0 mg / mL ), different reaction temperatures (20, 30, 50, 60, 70, 80℃), different reaction times (10, 20, 30, 45, 60, 120min) and the organic ratio of the reaction system (10%, 30 %, 50%, 70%, 90%) on the efficiency of the derivatization reaction.

[0055] by image 3 A. It can be seen that the peak area of ​​the derivatization product increases with the increase of the concentration of the derivatization reagent, until the concentration of 3-nitrophenylhydrazine hydrochloride is 500μg / mL (equivalent ...

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Abstract

The invention discloses a method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV / Vis. The method comprises the following steps: subjecting4-nitrobenzaldehyde to derivatization generation of a product with strong absorption in an ultraviolet-visible light zone in virtue of a nitrophenylhydrazine derivatization reagent; and with a reaction solution as a loading sample, determining the derivatization products of 4-nitrobenzaldehyde in the ultraviolet-visible light zone by using HPLC-UV / Vis based on the principle of reversed phase partition chromatography so as to realize qualitative or quantitative determination of 4-nitrobenzaldehyde. According to the invention, since the 4-nitrobenzaldehyde derivatization products based on the nitrophenylhydrazine derivatization reagent have obvious bathochromic shift effect due to generation of hydrazone bonds at nitro para-positions, the simple and universal method for determining 4-nitrobenzaldehyde through pre-column derivatization HPLC-UV / Vis is established. Methodological verification results show that the method has good specificity.

Description

Technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to a method for determining 4-nitrobenzaldehyde by a derivatized HPLC-UV / Vis method, in particular to a derivatized HPLC-UV / Vis method for determining chloramphenicol or its preparation. -Nitrobenzaldehyde method. Background technique [0002] Genotoxic impurities (GTIs) are a special type of pharmaceutical impurities. Due to their potential human carcinogenic effects, they have attracted more and more attention from the pharmaceutical industry and drug regulatory agencies [1-5] . The Threshold of toxicological concern (TTC) for genotoxic impurities in drugs depends on the daily dose and exposure period of the drug [6-8] . The International Conference on Harmonization (ICH) M7 (step 2) of the International Conference on Harmonization of Technical Requirements for the Registration of Human Drugs proposes a staged TTC as follows: 120μg / day for medications with a duration of less t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74G01N2030/027
Inventor 郑枫罗岚刘晶柳文媛
Owner CHINA PHARM UNIV
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