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High performance liquid chromatography qualitative/quantitative analysis method for amidotrizoic acid active ingredient and application thereof

A high-performance liquid chromatography and quantitative analysis technology, which is applied in the field of drug analysis and detection, can solve the problems of large experimental errors and cumbersome operation of silver nitrate titration, and achieve the effects of ensuring production and quality, solving quality control problems, and ensuring quality

Active Publication Date: 2017-06-13
SHANGHAI NEW HUALIAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The first purpose of the present invention is to provide a qualitative and quantitative analysis method of high performance liquid chromatography of diatrizoic acid bulk drug which is convenient, quick, accurate and reliable, so as to solve the problems of cumbersome operation and large experimental error of the existing silver nitrate titration method The second object of the present invention is to provide a kind of high performance liquid chromatography qualitative and quantitative analysis method in the composition analysis of diatrizoic acid bulk drug and the application in the content determination of diatrizoic acid bulk drug, guarantee the production and quality of bulk drug

Method used

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  • High performance liquid chromatography qualitative/quantitative analysis method for amidotrizoic acid active ingredient and application thereof
  • High performance liquid chromatography qualitative/quantitative analysis method for amidotrizoic acid active ingredient and application thereof
  • High performance liquid chromatography qualitative/quantitative analysis method for amidotrizoic acid active ingredient and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1 adopts the method of literature to qualitatively detect diatrizoic acid and the raw material nitro substance and key intermediate of synthesizing diatrizoic acid

[0045] In the fifth issue of 2011 of "Chinese Medicine and Clinic", Ning Huiqing and others published a document titled "Determination of Diatrizoate Glumine Injection by High Performance Liquid Chromatography" to detect diatrizoic acid in the preparation. However, there is no description on the intermediates that may exist in the production. For this reason, the applicant uses the methods in the literature to detect the API and the possible related substances in the API, and the steps are as follows:

[0046] (1) Chromatographic conditions

[0047] Mobile phase flow rate: 1.0mL / min;

[0048] Column temperature: 30°C;

[0049] Injection volume: 5μL;

[0050] Detection wavelength: 238nm;

[0051] Chromatographic column: Agilent SB-C18 5μm 150×4.6mm;

[0052] Mobile equipotential elution: met...

Embodiment 2

[0058] Embodiment 2 Separation and detection of diatrizoic acid, the raw material nitro substance of synthetic diatrizoic acid, and key intermediates

[0059] (1) Chromatographic conditions

[0060] Mobile phase flow rate: 1.0mL / min;

[0061] Column temperature: 30°C;

[0062] Injection volume: 10μL;

[0063] Detection wavelength: 238nm;

[0064] Chromatographic column: Phenomenex Kinetex 5μm XB-C18 100A 150×4.6mm;

[0065] Mobile equipotential elution: acetonitrile:phosphoric acid water (pH=2.0)=30:70, isocratic elution for 20min.

[0066] (2) Calculation method

[0067] Continuous injection of resolution solution, iodide stock solution, amino stock solution, and nitro stock solution. According to the relative retention time and the ultraviolet absorption spectrum, the related substances that may exist in the raw material drug are qualitatively analyzed through the peak identification of the resolution solution, and the content of impurities in the resolution solution a...

Embodiment 3

[0071] The content determination of embodiment 3 diatrizoic acid crude drug

[0072] (1) adopt the chromatographic condition identical with embodiment 1, specifically as follows:

[0073] Mobile phase flow rate: 1.0mL / min;

[0074] Column temperature: 30°C;

[0075] Injection volume: 10μL;

[0076] Detection wavelength: 238nm;

[0077] Chromatographic column: Phenomenex Kinetex 5μm XB-C18 100A 150×4.6mm;

[0078] Mobile equipotential elution: acetonitrile:phosphoric acid water (pH=2.0)=30:70, isocratic elution for 20min.

[0079] (2) Calculation method

[0080] Diatrizoic acid content: W 试 =(A 试 m 对 ·W 对 ) / (A 对 m 试 )

[0081] In the formula:

[0082] A 对 - in the reference substance solution, the average value of the peak area of ​​diatrizoic acid;

[0083] A 试 -in the test solution, the average value of the area of ​​diatrizoic acid;

[0084] m 对 - the quality of the diatrizoic acid reference substance, in grams (g);

[0085] m 试 - the quality of diatrizoi...

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Abstract

The invention discloses a high performance liquid chromatography analysis method for an amidotrizoic acid active ingredient. A core-shell type chromatographic column is used for the high performance liquid chromatography, acetonitrile and phosphoric acid-water are used as mobile phases, and separation is performed in an isocratic elution manner, wherein the pH value of the phosphoric acid water solution is 2.0, and the volume ratio of the acetonitrile to the phosphoric acid-water is 30:70. The high performance liquid chromatography analysis method disclosed by the invention can quickly determine the amidotrizoic acid active ingredient content, and can also detect raw materials and key intermediates in synthesis; and the detection result is accurate and reliable, thereby ensuring the production and quality of the amidotrizoic acid active ingredient.

Description

technical field [0001] The present invention belongs to the field of drug analysis and detection, and specifically relates to a high-performance liquid chromatography qualitative and quantitative analysis method for diatrizoic acid bulk drug and its application. The high-performance liquid chromatography method is used for diatrizoic acid bulk drug, Component analysis of raw materials and key intermediates in the synthesis of diatrizoic acid raw materials and rapid determination of the content of diatrizoic acid raw materials. Background technique [0002] Diatrizoic acid (Diatrizoic acid, structural formula shown in the following formula), chemical name is 3,5-bis(acetylamino)-2,4,6-triiodo-benzoic acid, is a positive contrast agent for X-ray diagnosis, for preparation Application of diatrizoate meglumine, sodium diatrizoate or compound diatrizoate meglumine injection. It is mainly used for urography, but also for cardiovascular, cerebrovascular, peripheral blood vessel, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74
Inventor 潘仙华李勤勤王亚萍胡剑蔡依依莫怡慧曹阳柏挺华吉涛
Owner SHANGHAI NEW HUALIAN PHARMA
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