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

A MALDI-TOF-MS, fluoroquinolone technology, applied in the field of food safety testing, can solve the problems of tediousness, the greatest impact on test results, time-consuming and labor-intensive, etc., to improve the detection efficiency and save the effect of the pretreatment process.

Inactive Publication Date: 2014-04-23
张金玲
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  • Abstract
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  • Claims
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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 smal

Method used

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

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Embodiment

[0034] Embodiment, the MALDI-TOF-MS detection method of fluoroquinolones in milk, comprises the following steps:

[0035] Steps for preparing 8-hydroxyquinoline functionalized mesoporous molecular sieves:

[0036] Put the mesoporous molecular sieve SBA-15 in a muffle furnace at 550°C for 2 hours, the purpose of heating is to remove the template agent;

[0037] Weigh 1.0g of mesoporous molecular sieve SBA-15, put it in 10mL of toluene solution mixed with 8-hydroxyquinoline, the content of 8QSi is 0.32g, stir at 80°C for 24h, and then raise the temperature to 120°C within 10 minutes And kept for 24h, and then filtered, the filtered solid was washed with toluene, acetone, methanol and dichloromethane in sequence, and dried under vacuum to obtain SBA-15-8QSi, namely SBA-15-8 hydroxyquinoline.

[0038] MALDI-TOF-MS sample preparation steps:

[0039] Take 10 μL of milk and dilute it with 0.1% trifluoroacetic acid at a volume ratio of 1:100 to obtain the target sample; take 1 mg of...

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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 ...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N30/06
Inventor 张金玲李凯孙军田国宁赵晗
Owner 张金玲
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