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Detection method of nicarbazin

A nicarbazine and sample technology, applied in the field of high-phase liquid chromatography analysis, can solve problems such as insignificant effect, large damage to the chromatographic column, shortened service life of the chromatographic column, etc., and achieve simplified operation process, high detection sensitivity, and separation good effect

Active Publication Date: 2015-06-03
HUBEI ZHONGMU ANDA PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high polarity of HDP, the HDP chromatographic peak has no effective retention. In this document, acetic acid / ammonium acetate buffered saline solution is used to prolong the peak time by reducing the pH of the buffer, but the effect is not obvious
María M. et al. ([J].Talanta, 2011, 85:142–150) used the method of adding ion-pairing reagents to improve the retention of HDP. The disadvantage is that the ion-pairing reagents are more harmful to the chromatographic column, and the combination with the stationary phase produces irreversible Adsorption, which in turn affects the stationary phase active sites
Moreover, the ion-pairing reagent is difficult to wash off from the column, which will greatly shorten the service life of the column

Method used

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  • Detection method of nicarbazin
  • Detection method of nicarbazin
  • Detection method of nicarbazin

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Experimental program
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Embodiment 1

[0039] HDP and DNC are measured in embodiment 1 nicarbazine

[0040] The present embodiment relates to the detection of HDP and DNC in nicarbazine, and its specific steps are as follows: 1) drawing of HDP and DNC standard curve

[0041]Nicarbazine standard solution: take 50mg of nicarbazine control sample (DNC content 70.9%, HDP content 29.1%), dissolve with 15mL DMSO, and dilute to 50mL with the volume ratio of acetonitrile and water of 80:20 mixed diluent as stock solution A.

[0042] The chromatographic column was Agilent poroshell 120Bonus-RP (4.6×150mm, 2.7μm), the ultraviolet detection wavelength was 300nm, the column temperature was 40°C, and the injection volume was 1μL; the mobile phase was a mixture of water and acetonitrile, and the gradient elution procedure was as follows: From 0 to 8 minutes, the percentage of water gradually changes from 99% to 10%; from 8 to 16 minutes, the percentage of water gradually changes from 10% to 99%, and the flow rate is 0.8mL / min ...

Embodiment 2

[0048] The mensuration of free HDP in the nicarbazine of embodiment 2

[0049] This embodiment relates to the mensuration of free HDP in nicarbazine, and its specific steps are as follows:

[0050] According to the standard of the Ministry of Agriculture: take 0.50 g of the raw drug nicarbazine, accurately weigh it, place it in a 25 mL volumetric flask, add 20 mL of phosphate buffer (pH=7.0), shake for 10 min, and dilute to the scale, shake well, and immediately filter. Discard the initial filtrate, take the intermediate filtrate, accurately measure 5mL, place it in a 50mL volumetric flask, and mix it with acetonitrile:water mixture with a volume ratio of 80:20 to prepare a test sample solution.

[0051] Select the chromatographic condition identical with embodiment 1, the HDP peak area ( Figure 5 ), according to the standard curve, calculate the content of free HDP.

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Abstract

The invention relates to a method for simultaneously determining 4, 4-binitrodiphenyl urea and 2-hydorxyl-4, 6-dimethyl pyrimidine in veterinary drug nicarbazin. The method comprises the following steps: preparing a sample into a solution, injecting the solution into high performance liquid chromatograph for detecting, wherein the condition of the high performance liquid chromatograph is as follows: a chromatographic column filled with a bonded alkyl amide group is selected, the column temperature is 25-40 DEG C, and the sample size is 0.5-2 microliter; and selecting water and acetonitrile as a moving phase, and adopting gradient elution, wherein the programs are as follows: 0-8 minutes, 99-100% of water; 8-16 minutes, 10% of water; 16-17 minutes, 10-99% of water; the flow rate of the moving phase is 0.5-1.5mL / min, and the detection wavelength is 260-380nm; the theoretical plate number based on nicarbazin is not lower than 5000. The method has the advantages of high detection sensitivity, good separating effect, simplicity and convenience and the like.

Description

technical field [0001] The present invention relates to the analysis field of high-phase liquid chromatography, be specifically related to 4 in nicarbazine, 4,-dinitrodiphenyl urea (DNC) and 2-hydroxyl-4, the 6-dimethyl pyrimidine (HDP) detection. Background technique [0002] Nicarbazin (nicarbazin), also known as coccidiostat, was developed by the American Merck Company in 1955. It has high-efficiency, broad-spectrum anticoccidial activity, good preventive effect, and slow development of drug resistance. It is still the most effective anti-coccidian. One of the coccidiostats. The chemical name of nicarbazine is 4, 4 ， - An equimolar complex of dinitrodiphenylurea (DNC) and 2-hydroxy-4,6-dimethylpyrimidine (HDP), abbreviated as DNC·HDP, CAS: 330-95-0. The anti-coccidia effect of DNC alone is weak, and the anti-coccidia effect is the best when it forms a 1:1 molecular inclusion complex with HDP. Nicarbazine is a typical clathrate, its structural stability is much weaker ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 徐金雷赵梅仙刘宏伟齐鹏梁景乐宋敏马佳颖
Owner HUBEI ZHONGMU ANDA PHARMACEUTICAL CO LTD