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Method for quantitatively detecting FQs(fluroquinolones) in chicken manure

A fluoroquinolone, quantitative detection technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low recovery rate, high quantitative limit and high cost of analysis and determination technology, and achieve the effect of low analysis cost

Inactive Publication Date: 2014-08-06
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems that FQs in the complex matrix is ​​not easy to analyze and measure, and the recovery rate of the existing analysis and determination technology is low, the quantitative limit is high, and the cost is high. A kind of fluorescence detection method based on solid phase extraction-high performance liquid chromatography is established. For the analysis of 6 fluoroquinolones (FQs) in chicken manure: norfloxacin (NOR), ciprofloxacin (CIP), lomefloxacin (LOM), danofloxacin (DAN), enrofloxacin (ENR), sarafloxacin (SAR)

Method used

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  • Method for quantitatively detecting FQs(fluroquinolones) in chicken manure

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Experimental program
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Embodiment 1

[0036] Compared with 50% Mg(NO 3 ) 2 -2.5% NH 3 ·H 2 O, EDTA-Mcllvaine buffer (pH=4) and acetonitrile and other inorganic and organic extracts, methanol: acetic acid: water (6:1:3, V / V) and EDTA-Mcllvaine: acetonitrile (1:1, V / V) V) and other mixed extracts, and EDTA-Mcllvaine buffer and methanol: acetic acid: water (6:1:3, V / V) recovery rate of each target compound extraction. The results are shown in Table 1. It can be seen from the table that the use of the inorganic extract 50% Mg(NO 3 ) 2 -2.5% NH 3 ·H 2 O, EDTA-Mcllvaine buffer or organic extract acetonitrile, all can not effectively extract the target from the matrix; while using organic-inorganic mixed extract methanol: acetic acid: water (6:1:3, V / V), The extraction efficiency of target substances such as NOR and CIP is still low. When using EDTA-Mcllvaine buffer solution and methanol: water: acetic acid = 6:1:3 for compound extraction, the extraction efficiency can basically meet the requirements, but the amou...

Embodiment 2

[0045] Table 2 Comparison of recoveries and relative standard deviations of six FQs at different pH values ​​of extracts

[0046]

Embodiment 3

[0048] An example of the invention is listed below, and the present invention is further described in conjunction with data, but the present invention is not limited to this example.

[0049] Chicken manure samples came from 4 large-scale chicken farms in the suburbs of Beijing (chicken farm 1, chicken farm 2, chicken farm 3 and chicken farm 4) and 1 natural free range farm (chicken farm 5, the chicken farm Antibiotics such as FQs have not been used in the field). Use a stainless steel shovel to collect fresh chicken manure on the same day in the chicken house of the chicken farm, collect and mix it at multiple points in a chicken farm to form a chicken manure sample, and seal it away from light (each chicken farm sample is numbered No. 1, 2 in sequence) No. 3, No. 4, No. 5), brought back to the laboratory and stored at -10°C. Take an appropriate amount from the chicken manure sample, freeze-dry, crush and pass through a 2mm sieve, take 0.5±0.005g of ground and sieved sample ...

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Abstract

The invention discloses a detection and analysis method for quantitatively detecting six FQs (fluroquinolones) in chicken manure. The method comprises the steps as follows: (1) freezing and drying a chicken manure sample; (2) crushing and sieving the chicken manure sample; (3) adding EDTA-Mcllvaine and an acetonitrile mixed extracting agent, and performing vortex even mixing and ultrasonic treatment; (4) obtaining a supernatant serving as an extracting solution through centrifugation; (5) removing an organic solvent and filtering the extracting solution with a filter membrane; (6) subjecting a filtering solution to an HLB (hydrophilelipophilebalance) column, pumping the filtering solution from the column, cleaning the column with a 5% methanol solution, finally eluting a target antibiotic with methyl alcohol, and collecting an eluent; (7) drying the eluent, determining the volume with acetonitrile / 0.7% phosphoric acid, and fully dissolving and filtering the solution for quantitative detection. According to the method, simultaneous detection of the six FQs is realized, the method has the characteristics of low cost, easiness in operation and the like, an optional method for detecting the FQs type antibiotics in complex matrixes is provided, and the method is low in both detection limit and quantitation limit and high in recovery rate.

Description

technical field [0001] The invention relates to a method for detecting antibiotics in a complex matrix, in particular to a method for detecting six kinds of fluoroquinolones (FQs) antibiotics in chicken manure. Background technique [0002] Fluoroquinolones (FQs) antibiotics are a class of synthetic broad-spectrum antibacterial drugs, piperazinyl derivatives of quinolones, which inhibit bacterial DNA helicase II (topoisomerase II) and topoisomerase IV (topoisomerase IV) and affect the DNA replication process of bacteria. Due to its broad-spectrum anti-Gram bacteria activity and good oral absorption effect, FQs are widely used in the poultry and livestock breeding industry for the prevention and treatment of poultry and livestock diseases and as feed additives. According to the statistics of the World Health Organization, 90% of the total antibiotics consumed in the world every year are used in poultry farming. For example, the aquaculture industry in the United States uses...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 薛南冬刘博张石磊李发生陈宣宇孟磊
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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