MALDI-TOF-MS (Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry) detection method of fluoroquinolone medicines in milk

Abstract

The invention discloses an MALDI-TOF-MS (Matrix-Assisted Laser Desorption / Ionization Time-of-Flight Mass Spectrometry) detection method of fluoroquinolone medicines in milk. The method comprises the following steps: sieving 8-hydroxyquinoline by a functional mesoporous molecular sieve to obtain SBA (Santa Barbara Amorphous material)-15-8-hydroxyquinoline; diluting milk by trifluoroacetic acid to obtain a sample target object; dispersing the SBA-15-8-hydroxyquinoline in ethanol liquor and carrying out ultrasonic treatment to obtain suspension liquid; adding the suspension liquid into the sample target object, and naturally drying at room temperature to obtain an MALDI matrix thin layer; placing milk to be detected on the MALDI matrix thin layer, carrying out MALDI-TOF-MS analysis after a solvent is naturally evaporated, and dropping a sample and the matrix on a target plate in a mixed manner, and detecting after the target plate directly enters into the MALDI-TOF-MS, wherein a fuzzy pre-treatment process is canceled. When the residual amount of the fluoroquinolone medicines in milk exceeds 0.05mg / kg, 18 of 25 fluoroquinolone medicines in milk can be effectively detected, so that the detection efficiency is greatly improved so as to meet the demand on quick test and quick release of import and export products.

Description

technical field [0001] The invention relates to a detection method of fluoroquinolones in milk, in particular to a MALDI-TOF-MS detection method of fluoroquinolones in milk, which belongs to the technical field of food safety detection. Background technique [0002] In recent years, matrix-assisted laser adsorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) technology has been widely used in the determination of molecular weight and purity evaluation of peptides and proteins, such as bovine carbonic anhydrase, melittin, bovine insulin, bovine insulin B chain, short The determination process of bacitracin S, myoglobin, cytochrome C, trypsinogen, etc. is very simple, and MALDI-TOF-MS has become a routine method for protein molecular weight determination in some laboratories at home and abroad. In terms of mass spectrometry analysis of peptides and amino acids, DHB and CHCA are mostly used as MALDI matrices. [0003] At present, MALDI-TOF-MS is mostly used for ...

AI Technical Summary

Problems solved by technology

[0003] At present, MALDI-TOF-MS is mostly used for the analysis of macromolecular substances, but the actual composition of the analyte often also contains small molecular substances. Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) In the region, due to the ionization of the matrix itself, there are a large number of unexplained peaks in the mass spectrum of small molecule compounds

The existence of a large number of miscellaneous peaks produces a strong mass discrimination effect, making it difficult for those small molecular compounds that are not easily ionized to desorb and ionize molecular ions

[0004] Fluoroquinolone residues are usually detected by enzyme-linked immunosorbent assay or liquid chromatography-mass spectrometry. The pretreatment process of the above detection methods is the most time-consuming, labor-intensive and cumbersome link in the entire detection process of fluoroquinolone residues. is the link that has the greatest impact on the test results

At present, there are no research reports on the use of MALDI-TOF-MS to detect fluoroquinolone residues

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