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High performance liquid chromatography method for 3-nitrophthalic acid

A nitrophthalic acid, high performance liquid chromatography technology, applied in the field of high performance liquid chromatography analysis, can solve the problems of weak column retention, long running time, inability to be separated, etc., and achieve accurate and reliable results and easy operation. , the effect of simple operation

Inactive Publication Date: 2019-02-12
JIANGSU YONGAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 3-Nitrophthalic acid and 3-nitro-2-methylbenzoic acid are highly hydrophobic acidic substances, which are easily dissociated in neutral mobile phases, resulting in octadecylsilane-bonded silica gel as the The packing is weakly retained in the column and cannot be separated
The method requires tight pH control, harsh conditions and long run times

Method used

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  • High performance liquid chromatography method for 3-nitrophthalic acid
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  • High performance liquid chromatography method for 3-nitrophthalic acid

Examples

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Embodiment 1

[0021] The high performance liquid chromatography analysis method of 3-nitrophthalic acid comprises the following steps:

[0022] 1) 3-nitro-2-methylbenzoic acid is made into a sample solution whose concentration is 0.4g / L;

[0023] 2) Inject 20 μL of the sample solution into the liquid chromatograph;

[0024] 3) Using a C18 chromatographic column with a solution composed of methanol and phosphoric acid as the mobile phase, the volume ratio of methanol and phosphoric acid is 6:4, the flow rate is 1.2mL / min, the detection wavelength is 254nm, and the sensitivity is 0.2aufs;

[0025] The concentration of phosphoric acid is 0.1mol / L, and the pH is 2.8.

[0026] The column temperature of the C18 chromatographic column is 30° C., the C18 chromatographic column is a Kromnsil C18 chromatographic column, the column size of the Kromnsil C18 chromatographic column is 150 mm×4.6 mm, and the particle size in the Kromnsil C18 chromatographic column is 5 μm.

[0027] Such as figure 1 As ...

Embodiment 2

[0029] The high performance liquid chromatography analysis method of 3-nitrophthalic acid comprises the following steps:

[0030] 1) 3-nitro-2-methylbenzoic acid is made into a sample solution whose concentration is 0.4g / L;

[0031] 2) Inject 20 μL of the sample solution into the liquid chromatograph;

[0032] 3) Using C18 chromatographic column, using methanol and sulfuric acid solution as the mobile phase, the volume ratio of methanol and sulfuric acid is 6:4, the flow rate is 1.0mL / min, the detection wavelength is 254nm, and the sensitivity is 0.2aufs;

[0033] Wherein the concentration of sulfuric acid is 0.1mol / L, and the pH is 2.8.

[0034] The column temperature of the C18 chromatographic column is 30° C., the C18 chromatographic column is a Kromnsil C18 chromatographic column, the column size of the Kromnsil C18 chromatographic column is 150 mm×4.6 mm, and the particle size in the Kromnsil C18 chromatographic column is 5 μm.

[0035] Such as figure 2 As shown, it i...

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Abstract

The invention discloses a high performance liquid chromatography method for 3-nitrophthalic acid, comprising the following steps of: 1) preparing 2-Methyl-3-nitrobenzoic acid into a sample solution having a concentration of 0.4 g / L; 2) injecting 10-40 [mu]L of the sample solution into a liquid chromatography; 3) using a C18 chromatographic column, taking a solution composed of methanol and sulfuric acid as a mobile phase or taking a solution composed of methanol and phosphoric acid as a mobile phase, wherein the flow rate is 0.8-1.2 mL / min, the detection wavelength is 254 nm, and the sensitivity is 0.2 aufs. According to the high performance liquid chromatography method, the content of 3-nitrophthalic acid, 2-Methyl-3-nitrobenzoic acid and other impurities can be quickly and accurately determined, and the analysis time can be effectively shortened. The high performance liquid chromatography method has the advantages of simple and convenient operation, accurate and reliable result, therepeatability, the special property of separating different interferences, and is suitable for popularization.

Description

technical field [0001] The invention relates to a high performance liquid chromatography analysis method, in particular to a high performance liquid chromatography analysis method of 3-nitrophthalic acid. Background technique [0002] 3-nitrophthalic acid and 3-nitro-2-methylbenzoic acid are important intermediates in organic synthesis, which can be used to synthesize medicines, dyes, photosensitive materials, crop protection agents, etc., and their preparation is by using 3- Nitro-phthalylene is oxidized to form a mixture of the two, and then separated. Contains 3-nitro-2-methylbenzoic acid and other impurities in 3-nitrophthalic acid. Therefore, it is of great significance to realize the separation and accurate quantification of the two. [0003] 3-Nitrophthalic acid and 3-nitro-2-methylbenzoic acid are highly hydrophobic acidic substances, which are easily dissociated in neutral mobile phases, resulting in octadecylsilane-bonded silica gel as the Packing materials are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 陈夕鹏王晓军袁爱菊
Owner JIANGSU YONGAN CHEM CO LTD
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