Pretreatment method for determining quinolone residues in animal-derived products

Abstract

The invention relates to a pretreatment method for determination of quinolone residues in animal-derived products, which comprises the following steps: weighing a proper amount of a sample, putting the sample into a centrifuge tube, adding a formic acid-acetonitrile solution, and homogenizing with a homogenizer; after homogenizing, adding anhydrous sodium sulfate into the centrifuge tube, and uniformly mixing; centrifuging, and extracting supernatant for the second time; adding acetonitrile saturated n-hexane into the supernatant, shaking, discarding the upper-layer solution, and transferringthe lower-layer extracting solution into a heart-shaped bottle; adding n-propanol or isopropanol into a heart-shaped bottle, and then carrying out rotary evaporation; adding a formic acid-acetonitrilesolution to dissolve residues, filtering, fixing the volume, transferring the fixed solution into a 10mL centrifuge tube after fixing the volume, adding acetonitrile saturated n-hexane, performing vortex mixing, performing low-temperature high-speed centrifugation, taking the lower-layer liquid, and detecting on an organic filter membrane machine. According to the method, the phenomenon that thesolution in the heart-shaped bottle is exploded and boiled during rotary evaporation is reduced, the problem that the nitrogen blowing time is too long is solved, and the phenomenon that white particles are separated out of the high-fat sample final solution is avoided.

Description

Technical field: [0001] The invention relates to the technical field of food detection, in particular to a pretreatment method for the determination of quinolone residues in animal source products. Background technique: [0002] The National Standard of the People’s Republic of China. Determination of Quinolone Residues in Products of Animal Origin. Liquid Chromatography-Tandem Mass Spectrometry (GB / T 20366-2006). In the extraction and purification of samples, it is mentioned that "5.0g of sample is added with formic acid-acetonitrile twice. After extraction, the supernatant was collected and washed with acetonitrile-saturated n-hexane by shaking. After layering, the lower liquid was rotary evaporated to near dryness. After nitrogen was blown to dryness, the volume was fixed to 1.0 mL for machine testing." [0003] The previous treatment method was too general, and there were the following problems: 1. Rotary steaming at 40°C would easily cause the liquid in the bottle to boil, res...

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Problems solved by technology

[0003] The previous treatment method was too general, and there were several problems: 1. Rotary steaming at 40°C would easily cause the liquid in the chicken heart bottle to boil, resulting in a low recovery rate; 2. Animal-derived foods with high water content, A large amount of liquid will remain after the rotary evaporation, which will cause the nitrogen blowing time to be too long and reduce the detection efficiency; 3. For samples with high oil content, white particles will precipitate after constant volume, which may block the liquid quality system.