Analysis of p-chloro-o-nitroacetoacetanilide by high performance liquid chromatography

Abstract: o-chloronitrobenzene, molecular formula is C6H4ClNO2, light yellow needle crystal. Insoluble in water, soluble in ethanol, ether and benzene. It is an important intermediate for pesticides, dyes and medicines, and can also be used as a raw material for rubber accelerator M.

P-chloro-o-nitroacetoacetanilide is an intermediate in the synthesis of pesticides quinquine, quinoxaline, and lencon. This article uses high performance liquid chromatography internal standard method to determine the content of p-chloro-o-nitroacetoacetanilide. The effective separation of chloro-o-nitroacetoacetanilide and its impurities is achieved, the operation is simple and fast, the results are reproducible, and the quantitative is accurate.

1. Reagents and solutions

Methanol: chromatographically pure, filtered through 0.45um filter membrane before use;

Water: freshly distilled double distilled water;

Tetrahydrofuran: analytically pure;

Pyrimethanil: No interfering impurity peaks;

Standard sample of p-chloro-o-nitroacetoacetanilide: known mass fraction> 94.6%.

2. Instruments

LC-3000 high performance liquid chromatograph; with variable wavelength ultraviolet detector;

LDT230 column thermostat;

All Chinese system anti-control software includes chromatographic workstation;

Chromatography column: C18 (150 mmx4.6mmx5um)) stainless steel column;

1 / 100,000 electronic balance;

Ultrapure water system;

Filter: The pore size of the filter membrane is about 0.45um.

3. Operating conditions of liquid chromatography

Mobile phase: methanol water = 65 35 (v / v); flow rate: 1.0 mL / min; column temperature: 30 ° C; detection wavelength: 252 nm; injection volume: 5 uL; retention time: p-chloro-o-nitroacetoacetanilide 6 min, pyrimethanil 11.1 min. The above liquid chromatography operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating parameters can be adjusted appropriately. In order to get the best results.

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