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Multi-detection method of residual of cephalo-type drugs in milk product

A detection method, the technology of cephalosporins, is applied in the field of detection of drug residues in animal-derived foods, which can solve the problems of cumbersome antibody preparation steps, high detection limit, and difficulty in accurate quantitative detection, so as to facilitate effective monitoring and improve efficiency , The effect of shortening the processing time

Active Publication Date: 2015-12-02
山东世通检测评价技术服务有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent (CN200910085945.7) discloses an enzyme-linked immunosorbent assay kit for detecting cephalosporins and its application. The enzyme-linked immunosorbent assay is used to detect the residues of cephalosporins veterinary drugs, and the residual amount can only be roughly judged by the absorbance value. Antibody preparation The steps are cumbersome, the detection limit is high, and it is not easy to be used for accurate quantitative detection

Method used

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  • Multi-detection method of residual of cephalo-type drugs in milk product
  • Multi-detection method of residual of cephalo-type drugs in milk product
  • Multi-detection method of residual of cephalo-type drugs in milk product

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Embodiment 1

[0063] Present embodiment is the mensuration of cephalosporin antibiotic residue in liquid milk, consists of the following steps:

[0064] (1) Sample pretreatment

[0065] Measure 5 mL of liquid milk sample, put it into a 50 mL centrifuge tube, add 15 mL of acetonitrile, ultrasonically oscillate (5 seconds, 5 seconds apart, 60 cycles), centrifuge at 5000 rpm for 10 min, draw the supernatant into the test tube, blow dry with nitrogen, Add an equal volume of methanol-0.1% formic acid solution (v / v, 3 / 7) to redissolve, add 2ml of n-hexane to degrease, shake, centrifuge at 5000rpm for 10min, discard n-hexane, and filter through 0.45μm and 0.22μm membranes Follow-up HPLC analysis;

[0066] (2) Detection condition setting

[0067] The high performance liquid chromatography conditions used in the experiment

[0068] Agilent1100 High Performance Liquid Chromatograph

[0069] Agilent (C18, 4.6x250, 5μm) ZORBAX EclipsePlus reversed-phase column

[0070] Mobile phase: A-methanol, B-...

Embodiment 2

[0098] The present embodiment is the determination of cephalosporin antibiotic residues in solid milk, which consists of the following steps:

[0099] (1) Sample pretreatment

[0100] Measure 1g of solid milk sample, add 4ml of pure water, mix well, place in a 50mL centrifuge tube, add 20mL of acetonitrile, ultrasonically oscillate (5 seconds, interval 5 seconds, 60 cycles), centrifuge at 5000rpm for 10min, absorb the supernatant Put it into the test tube, dry it with nitrogen, add methanol-0.1% formic acid solution (v / v, 4 / 6) to redissolve, add 2.5ml n-hexane to degrease, oscillate, centrifuge at 5000rpm for 10min, discard n-hexane, successively wash through 0.45μm and 0.22μm membrane filter before high-performance liquid chromatography analysis;

[0101] (2) Detection condition setting

[0102] The high performance liquid chromatography conditions used in the experiment

[0103] Agilent1100 High Performance Liquid Chromatograph

[0104] Agilent (C18, 4.6x250, 5μm) ZORBAX...

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Abstract

The invention belongs to the technical field of detection of residual of drugs in an animal source food, and relates to a method for determining the residual quantity of cephalo-type drugs in a milk product through a high performance liquid chromatograph. The method comprises the steps of sample pre-extraction, standard curve drafting and apparatus detection analysis, the detection method is a multi-detection method carried out by using high performance liquid chromatography, and detected drugs comprise cefoperazone, cefotaxime, ceftriaxone and cephalothin. The cefoperazone detection limit of the method is 0.26mg / Kg, the cefotaxime detection limit of the method is 0.01mg / Kg, the ceftriaxone detection limit of the method is 0.10mg / Kg, and the cephalothin detection limit of the method is 0.07mg / Kg; the method has good linear relationship in an addition concentration range of 1-50mg / kg, and the recovery rate is 90-105%; and the intra-batch relative standard deviation is not greater than 15%, and the inter-batch relative standard deviation is not greater than 20%. The method has the advantages of short analysis time, low detection limit, high precision and multi-detection, and is of great significance to accurately monitor the residual quantity of the cephalo-type drugs in milk.

Description

technical field [0001] The invention belongs to the technical field of detection of drug residues in animal-derived foods, and relates to a method for measuring the residual amount of cephalosporins in milk products by using a high-performance liquid chromatography. Background technique [0002] With the rapid development of animal husbandry in my country, veterinary drugs have played a significant role in reducing the morbidity and mortality of livestock and poultry, promoting animal production, improving the quality of animal meat products and improving feed utilization, and have become an important support for modern animal husbandry. Cephalosporins belong to β-lactam antibiotics, which have the characteristics of penicillinase resistance, high curative effect, low toxicity, less allergic reaction, and broad antibacterial spectrum, and can effectively inhibit the growth and reproduction of bacteria. In animal husbandry, cephalosporin antibiotics are widely used in the pre...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 孙海新黄金发张慧许娜孙丕春
Owner 山东世通检测评价技术服务有限公司
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