Method for determining fluoroquinolone drug residual in beef

A technology for the determination of fluoronoquinone and its method, which is applied in the field of determination of drug residues in meat products, can solve the problems of drug abuse, adverse reactions, irrational drug use, etc., and achieves short time consumption, good extraction effect, precision and accuracy Good results

Inactive Publication Date: 2015-02-04
LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Any drug has side effects, and fluoroquinolones are no exception. Due to the wide application of fluoroquinolones, irrational drug use and drug abuse often occur. The adverse reactions of fluoroquinolones mainly occur in humans, while animals have little reaction. However, drug residues in animals can be transmitted through the food chain, which can also cause adverse reactions in humans and affect human health. Therefore, the detection of fluoroquinolone residues in animals has attracted more and more attention

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  • Method for determining fluoroquinolone drug residual in beef

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Ultrasonic extraction:

[0034] Accurately weigh 2.0±0.01 g of the sample, put it into a 50mL conical flask with a stopper, add a certain amount of extraction solution as the extraction solution, cover the stopper tightly, and place it on an ultrasonic cleaner for extraction. The extract was centrifuged immediately, and the supernatant was purified by a solid-phase extraction column, eluted with methanol, and the eluate was blown dry with a nitrogen blower at 60°C. Finally, it was dissolved with mobile phase, filtered into the sampling bottle, and measured by high performance liquid chromatography.

[0035] 2. Liquid chromatography instrument method:

[0036] The mobile phase is citric acid / ammonium acetate buffer-acetonitrile (V:V=82:18), the flow rate is 1.0mL / min, the column temperature is 25°C, the injection volume is 20μl, the excitation wavelength of the fluorescence detector is 280nm, and the emission wavelength is 450nm .

[0037] 3. Optimization of ...

Embodiment 2

[0050] The determination method of fluoronoquinone drug residues in beef, comprises the following steps:

[0051]1) Accurately weigh 1.99g of beef sample, put it into a 50mL conical flask with a stopper, add 2.5mL of ultrasonic extraction solvent per 1g of beef sample, cover the stopper tightly and place it on an ultrasonic cleaner Carry out extraction, extraction time is 5min, obtains extract, and ultrasonic extraction solvent is the acetonitrile-10% trichloroacetic acid solution that volume ratio is 30:70;

[0052] 2) Immediately centrifuge the extract obtained in step 1) after the extraction, the centrifugation speed is 8000r / m, the centrifugation time is 6min, and the centrifuged supernatant is obtained;

[0053] 3) Purify the centrifuged supernatant obtained in step 2) through a reversed-phase solid-phase extraction column, and then elute with 5ml of methanol to obtain the eluent; the reversed-phase solid-phase extraction column must first be activated with 3ml of methano...

Embodiment 3

[0056] The determination method of fluoronoquinone drug residues in beef, comprises the following steps:

[0057] 1) Accurately weigh 2.01g of beef sample, put it into a 50mL conical flask with a stopper, add 12.5mL of ultrasonic extraction solvent per 1g of beef sample, close the stopper tightly and place it on an ultrasonic cleaner Carry out extraction, extraction time is 25min, obtains extract, and ultrasonic extraction solvent is the acetonitrile-10% trichloroacetic acid solution that volume ratio is 30:70;

[0058] 2) Immediately centrifuge the extract obtained in step 1) after the extraction, the centrifugation speed is 8000r / m, the centrifugation time is 6min, and the centrifuged supernatant is obtained;

[0059] 3) Purify the centrifuged supernatant obtained in step 2) through a reversed-phase solid-phase extraction column, and then elute with 5ml of methanol to obtain the eluent; the reversed-phase solid-phase extraction column must first be activated with 3ml of meth...

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Abstract

The invention discloses a method for determining fluoroquinolone drug residual in beef. The method comprises the following steps: accurately weighing a beef test sample, adding an ultrasonic extracting solvent for extracting, centrifuging the extract, purifying the obtained centrifuged liquid supernatant by use of a reverse solid-phase extraction column, next, eluting by use of 5mL of methanol, drying the obtained eluate by use of a nitrogen blowing instrument at the temperature of 60 DEG C, dissolving the dried eluate in a moving phase, filtering the solution by use of a 0.22-micron filter membrane and putting the filtrate into a sample injection bottle, and finally, determining the filtrate by use of a high performance liquid chromatograph with a fluorescence detector. The method for determining the fluoroquinolone drug residual in the beef has the beneficial effects that two main factors, namely the extraction time and the extract dosage, are optimized so that the optimal ultrasonic extraction time and the optimal extract material ratio can be obtained, and the method has the advantages of good extraction effect, short time consumption, good sensitivity, precision and accuracy and the like, and is suitable for quick detection on the fluoroquinolone drug residual in the beef samples.

Description

[0001] technical field [0002] The invention relates to a method for determining drug residues in meat products, in particular to a method for determining fluoroquinolone drug residues in beef. Background technique [0003] Fluoroquinolones are a class of antibacterial drugs whose mechanism of action is to inhibit bacterial DNA helicase and hinder DNA replication. Fluoroquinolones have good antibacterial activity against G-bacteria, including Pseudomonas aeruginosa, and have certain antibacterial activity against G+ cocci, especially for drug-resistant G-bacteria, which can still show sensitivity. It is clinically used to treat urinary tract, intestinal tract, respiratory tract, skin and soft tissue, abdominal cavity, bone and joint infections. Any drug has side effects, and fluoroquinolones are no exception. Due to the wide application of fluoroquinolones, irrational drug use and drug abuse often occur. The adverse reactions of fluoroquinolones mainly occur in humans, whi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
Inventor 熊琳高雅琴李维红郭天芬杨晓玲
Owner LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS
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