QuEChERS-triple quadrupole tandem mass spectrometry method for detecting residues of four nitrofuran metabolites in shrimp flesh

Abstract

The invention discloses a QuEChERS-triple quadrupole tandem mass spectrometry method for detecting residues of four nitrofuran metabolites in shrimp flesh. A sample is treated by using a QuEChERS method, and in combination with triple quadrupole tandem mass spectrometry detection, the method comprises the following steps: preparing a standard solution, using a sample matrix solution to prepare a mixed standard curve solution; carrying out hydrolysis and derivatization, homogenizing and homogenating the sample, deriving 2-nitrobenzaldehyde and hydrochloric acid, and keeping in dark place for 16 h; carrying out extraction and purification, after vibrating extraction of a derivative solution through 5% formic acid acetonitrile, using the QuEChERS method for purification, using a liquid chromatogram-mass spectrometer for detection, and quantifying with an internal standard method. Traditional liquid-liquid extraction is replaced by using QuEChERS purification, the influence on pH and easily emulsified protein in liquid-liquid extraction is overcome, other impurities in shrimp flesh matrix can be removed effectively, the recovery rate, repeatability, sensitivity and detection limit meet the requirement of national standard, and the method has the characteristics of being high in speed, simple and convenient, high in efficiency, low in cost, environmentally-friendly and the like.

Description

technical field [0001] The invention relates to the technical field of veterinary drug residue detection, in particular to a QuEChERS-triple quadrupole tandem mass spectrometry method for detecting residues of four nitrofuran metabolites in shrimp meat. Background technique [0002] China is the world's largest producer of prawn farming. In recent years, my country's export shrimp products have maintained a rapid growth rate, but the number of notifications from official agencies has also increased relatively, especially the residues of nitrofuran drugs that exceed the standard. universal. Nitrofuran is a typical synthetic broad-spectrum antibiotic drug, which is widely used in the prevention and control of diseases in livestock, poultry and aquatic products. Studies have shown that this type of drug is carcinogenic and mutagenic. Many countries, including China, The use of nitrofurans is expressly prohibited. However, due to its low price and good medicinal properties, the...

AI Technical Summary

Problems solved by technology

However, the development of pretreatment technology is relatively slow. If the sample pretreatment is not extracted well, it will cause great interference to the detection.

At present, the pretreatment of metabolites of nitrofuran drugs is mainly liquid-liquid extraction and solid-phase extraction. These methods are not only costly, consume a lot of reagents, are likely to cause environmental pollution, and are cumbersome to operate.

The national standard "Announcement No. 783-1-2006 of the Ministry of Agriculture" adopts ethyl acetate liquid-liquid extraction operation, and the furan components are greatly affected by the change of pH value; at the same time, samples with high protein content such as shrimp are easy to extract after extraction. Emulsification occurs, and protein needs to be removed again, which makes the pretreatment operation more cumbersome and complicated

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