Method for detecting cyanoacetamide by reversed-phase high performance liquid chromatography

Abstract

The invention relates to the technical field of detection and analysis, in particular to a method for detecting cyanoacetamide by reversed-phase high performance liquid chromatography. According to the method, the following chromatographic conditions are adopted: a chromatographic column is an Agilent ZORBAX Eclipse XDB-CN liquid chromatographic column (4.6 mm * 250 mm, 5 [mu] m); a mobile phase is an acetonitrile-ammonium formate volatile buffer solution; the flow rate is 0.5 mL / min; the detection wavelength is 200 nm; the column temperature is 40 DEG C; the sample size is 5 [mu] L; the detector adopts a diode array detector. According to the method, the quality of cyanoacetamide can be better controlled, the analysis accuracy is improved, and the accuracy is high; the detection linearityand range, the recovery rate, the precision and other tests are good.

Description

technical field [0001] The invention relates to the technical field of detection and analysis, in particular to a method for detecting cyanoacetamide by reverse-phase high-performance liquid chromatography. Background technique [0002] Cyanoacetamide is a commonly used raw material for organic synthesis, used in the synthesis of malononitrile, electroplating solution and pesticide triamterene, aminopterin. As an important synthetic intermediate, malononitrile can be generated by dehydration; the fungicide 2,2-dibromo-2 cyanoacetamide can be obtained by bromination; and substituted pyridine compounds can be obtained after cyclization with ethyl trifluoroacetoacetate. The synthesis results in the insecticide flonicamid; similarly, cyanoacetamide is also one of the important raw materials for the fungicide fludioxonil. Its structural formula is as follows: [0003] [0004] As an important raw material in the chemical industry, cyanoacetamide is generally used to detect t...

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Problems solved by technology

Quantitative detection can be achieved with normal phase liquid chromatography, but the operation is more complicated, which brings inconvenience to the analysis work, especially when monitoring the reaction status through liquid phase, it is not timely and intuitive, and the detection cycle is long, which is not only time-consuming, but also impossible. Accurately and intuitively reflect the status of the reaction, and often because the polarity of the product or another raw material is small, normal phase liquid chromatography cannot effectively track

Wei Yang et al. used high-performance liquid phase phase ODS column, C18 or C8 for detection, but because cyanoacetamide is highly polar, the retention on the reverse phase ODS column is very weak, and it often appears simultaneously with inverted peaks, solvent peaks, and impurity peaks. peak, it is difficult to achieve accurate quantitative detection of cyanoacetamide

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