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Milk and milk product tetracycline antibiotic residual quantity checking method

A technology of tetracyclines and detection methods, applied in the field of analysis, can solve the problems of high detection limit and long detection time of tetracycline antibiotics, reduce the probability of false positive (negative) detection results, short detection time and high sensitivity Effect

Active Publication Date: 2008-10-22
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used detection method of tetracycline antibiotics in milk and milk products is mainly high performance liquid chromatography, using high performance liquid chromatography (ultraviolet detector) to determine the residual amount of tetracycline antibiotics, but using this method, the detection time is longer Generally, it takes about 30 minutes to complete the detection of a sample, and the detection limit of tetracycline antibiotics by high performance liquid chromatography is relatively high (generally higher than 10 μg / kg)

Method used

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  • Milk and milk product tetracycline antibiotic residual quantity checking method
  • Milk and milk product tetracycline antibiotic residual quantity checking method
  • Milk and milk product tetracycline antibiotic residual quantity checking method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1 The content of oxytetracycline, tetracycline and aureomycin in milk was determined by ultra-high performance liquid chromatography-electrospray tandem triple quadrupole mass spectrometer.

[0060] 1) Preparation of standard solution:

[0061] Accurately weigh 10 mg each of oxytetracycline, tetracycline, and chlortetracycline standard substances, use methanol to make up volume in a 10 mL brown volumetric flask, and mix well to obtain a standard with the concentration of oxytetracycline, tetracycline, and chlortetracycline being 1.00 mg / mL. The stock solution should be stored in a -18°C freezer in the dark for at least 4 weeks. When in use, dilute to 100ng / mL, 50ng / mL, 20ng / mL, 1ng / mL, 0.1ng / mL standard solution.

[0062] 2) Preparation of reagents:

[0063] (a) Preparation of extract:

[0064] 0.2mol / L disodium hydrogen phosphate solution: Accurately weigh 28.41g of disodium hydrogen phosphate, dissolve in water, and dilute to 1000mL.

[0065] 0.1mol / L citr...

Embodiment 2

[0095] Example 2 The contents of oxytetracycline, tetracycline and aureomycin in yogurt were determined by ultra-high performance liquid chromatography-electrospray tandem triple quadrupole mass spectrometer.

[0096] 1) Preparation of standard solution:

[0097] Accurately weigh 10 mg each of oxytetracycline, tetracycline, and chlortetracycline standard substances, use methanol to make up volume in a 10 mL brown volumetric flask, and mix well to obtain a standard with the concentration of oxytetracycline, tetracycline, and chlortetracycline being 1.00 mg / mL. The stock solution should be stored in a -18°C freezer in the dark for at least 4 weeks. When in use, dilute to 50ng / mL, 20ng / mL, 10ng / mL, 1ng / mL, 0.1ng / mL standard solution.

[0098] 2) Preparation of reagents:

[0099] (a) Preparation of extract:

[0100] 0.2mol / L disodium hydrogen phosphate solution: Accurately weigh 28.41g of disodium hydrogen phosphate, dissolve in water, and dilute to 1000mL.

[0101] 0.1mol / L c...

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Abstract

The invention relates to a method for detecting the residue amount of terracycline antibiotics in milk and dairy products. The method utilizes an ultra performance liquid chromatography - electrospray tandem triple quadrupole mass spectrometer to determine the residue amount of the terracycline antibiotics. The method is as follows: a sample is extracted from Na2EDTA-McIlvaine buffer solution (pH4.0); proteins are removed by trichloroacetic acids; a columella is extracted through an HLB solid phase and then purified and enriched; the sample is separated by a chromatographic column, with the column temperature of 30 DEG C; gradient elution is performed by utilization of water solution (v / v) which contains 0.1 percent of methanoic acids and acetonitrile as a moving phase; and quantitative detection is performed by adoption of the multi-reaction monitoring means. The detection limit of instruments is between 1.0 and 2.0 mu g / kg; a related coefficient r reaches over 0.999 within the linear range of between 1 and 100 mu g / kg; and the recovery rate is between 81.7 and 100.7 percent (the addition levels are 10 mu g / kg, 50 mu g / kg and 100 mu g / kg). The method has the advantages of quickness, accuracy, high sensitivity and wide application scope.

Description

technical field [0001] The invention relates to a method for detecting the antibiotic content in milk and dairy products, in particular to a method for detecting the residual amount of tetracycline antibiotics in milk and dairy products, and belongs to the field of analysis technology. Background technique [0002] Tetracycline antibiotics are sensitive to most Gram-positive and negative bacteria, and are mainly used for the prevention and treatment of brucellosis, anthrax, Escherichia coli, acute respiratory infection, mastitis, etc., because of their broad-spectrum antibacterial effect And the cheap price has become the main variety of commonly used veterinary antibiotics in recent years. However, the drug will remain in the livestock and poultry body. The tetracyclines in the milk have the greatest damage to human lungs, gastrointestinal tract, kidneys, skin and bones, especially the teeth of children, which can affect the growth of fetal bones and teeth, causing dentin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/00G01N33/15G01N30/06
Inventor 闫宁环陈伟袁汉成李梅常建军
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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