Method for detecting malachite green, leuco malachite green, crystal violet and leuco crystal violet in aquatic products

Abstract

The invention, which belongs to the technical field of aquatic product quality safety detection, relates to a method for efficiently detecting malachite green, leuco malachite green, crystal violet and leuco crystal violet residues in aquatic products. The detection method is a high performance liquid chromatography-mass spectrometry combined detection method. According to the detection method, isotope corresponding to a target compound is taken as an internal standard, and a to-be-detected product is extracted by extracting solution acetonitrile, the extracted product is purified by a neutralalumina solid-phase extraction column and the purified product is filtered by a 0.22-micron microfiltration membrane and then the substance is detected by a high performance liquid chromatography-mass spectrometer. According to the detection technology, different aquatic products are tested, the recovery rate can reach 85%-120%, the detection limits of four detection indexes can reach 0.5 microgram /kg, and the standard curve r value is over 0.99. Compared with the existing detection method, the method has the advantages of few reagents, low pretreatment cost, simple steps, easiness in operation and complete detection parameters, and is very suitable for large-batch detection of aquatic products.

Description

technical field [0001] The patent of the invention belongs to the technical field of aquatic product quality and safety detection, and relates to a method for efficiently detecting residual amounts of malachite green, leuco malachite green, crystal violet, and leuco crystal violet in aquatic products. Background technique [0002] Malachite green and crystal violet are artificially synthesized triphenylmethane basic industrial dyes. They are widely used in the breeding process of aquatic products because they can be sterilized and sterilized and are cheap. They are mainly used to prevent and treat aquatic animals. Mildew, strontium mildew, parasitic disease, small melon worm disease, ringworm disease, oblique tube worm disease, third-generation worm disease and some other bacterial diseases, etc., can also be used for the input of aquatic products and the process of temporary breeding of aquatic products , to prolong the survival time of aquatic products, especially fish pro...

AI Technical Summary

Problems solved by technology

The main principle of GB / T 20361-2006 high-performance liquid chromatography detection method is to reduce malachite green and crystal violet to their corresponding metabolites leuco malachite green and leuco crystal violet with potassium borohydride, acetonitrile ammonium acetate buffer mixture Extraction, dichloromethane liquid-liquid extraction, solid-phase extraction column purification and detection on the machine. The pretreatment of this method is complicated and tedious, which is easy to cause losses. There are many kinds of reagents used, and the efficiency is low when dealing with large-scale sample detection.

The main principle of GB / T 19857-2005 liquid chromatography tandem mass spectrometry and high performance liquid chromatography is to use acetonitrile ammonium acetate buffer mixture to extract, acetonitrile to extract again, the solution is distributed to the dichloromethane layer through the neutral alumina column and cationic After the solid-phase column is purified and tested on the machine, this method has high detection sensitivity, but it also has the problem of complex and cumbersome pretreatment, and there are many reagents and pretreatment instruments used, the cost of pretreatment is high, and the processing process requires relatively high professional skills for professional testing personnel. High, the quality of the test results is difficult to control, SC / T 3021-2004 can only detect malachite green and leuco malachite green in aquatic products, and does not test crystal violet and leuco crystal violet

In addition, for the detection methods of malachite green and crystal violet, there is another type of rapid detection technology based on enzyme standard method and enrichment method, such as cloud point extraction technology and synergistic extraction technology, etc. These methods do not require large instruments Auxiliary detection, and the speed is fast, usually the result can be obtained within half an hour, but the disadvantage is that the quantification is not accurate, the detection limit is high, and only preliminary screening can be carried out, and it is difficult to meet the national standard requirements

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