Method for simultaneously detecting multi-kind pesticide residues in bee products

A technology of bee products and agricultural and veterinary drugs, applied in the field of simultaneous detection of multiple types of agricultural and veterinary drug residues in bee products, to achieve the effects of improved analysis efficiency, good selectivity, and high sensitivity

Inactive Publication Date: 2009-02-04
中华人民共和国江苏出入境检验检疫局
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, when enterprises export animal-derived products such as bee products and aquatic products, they need to conduct a large amount of testing and monitoring. Taking honey as an example, an enterprise needs to pay more than 10,000 yuan to complete a complete set of drug residue testing. One of the burdens of export enterprises

Method used

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  • Method for simultaneously detecting multi-kind pesticide residues in bee products
  • Method for simultaneously detecting multi-kind pesticide residues in bee products
  • Method for simultaneously detecting multi-kind pesticide residues in bee products

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The detection of agricultural and veterinary drug residues in honey sample of embodiment 1

[0020] Accurately weigh 5.00g (±0.05g) of honey sample into a 50mL centrifuge tube, add 10mL of 2% trichloroacetic acid solution, vortex and mix, then add 5mL of 0.5mol / L sodium acetate solution to control the concentration of the solution. pH value is 4.5; after centrifugal filtration, add to the HLB solid phase extraction column activated by 5ml methanol and 5mL water, the flow rate is controlled at 1-2d / s, after the flow is over, wash the centrifuge tube and the storage tube with 5mL water and pass through the column, Discard all effluent. Under a negative pressure of 65kPa, vacuum dry for 10min, and finally elute with 0.2% oxalic acid-methanol, collect the eluate in a 10mL test tube, dry the extraction column with a nitrogen blower at 45°C, and use 30% The methanol solution was adjusted to 1.0 mL, passed through a filter membrane with an average pore size of 0.45 μm, and th...

Embodiment 2

[0023] The pesticide and veterinary drug residue detection of embodiment 2 royal jelly samples

[0024] Accurately weigh 2.00g±0.05g of royal jelly or 1.00g of dry powder into a 50mL centrifuge tube, add 10mL of 4% perchloric acid solution, vortex and mix, then add 5mL of 0.5mol / L sodium phosphate solution to control the pH value of 7.4; after centrifugal filtration, add a C18 solid-phase extraction column activated by 5ml methanol and 5mL water, and control the flow rate at 1-2d / s. Remove all effluent. Under a negative pressure of 65kPa, vacuum dry for 10min, and finally elute with 2g / L oxalic acid-methanol, collect the eluate in a 10mL test tube, and dry the extraction column with a nitrogen blower at 45°C , use 30% methanol solution to dilute to 1.0 mL, pass through a filter membrane with an average pore size of 0.45 μm, collect the filtrate into a sample bottle for liquid chromatography-mass spectrometer determination. Table 4 shows the recovery detection results of nega...

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Abstract

The present invention relates to a method of simultaneously detecting a plurality of agro-veterinary drug residues in bee products. The extracted liquid trichloroacetic acid or perchloric acid and the extracted liquid acetate, phosphate or borate solution are added into a sample; the pH value is controlled between 4.5 and 9.0; the mixed solution is centrifuged, the filtrate is added into a solid phase extraction column to be extracted, the extraction column is eluted and dried, the column is washed by oxalic acid-methanol solution, the volume of the eluent is defined by the aqueous solution of methanol, the eluent is added into liquid chromatography-tandem mass spectrometry to be analyzed and tested, the acquired chromatographic peak is contrasted with the known standard chromatographic peak of the drug, and according to the retention time and the abundance of the mass spectrum ions, the specific name of the detected drug is determined. The method only requires one pre-treatment of the sample, and thus can simultaneously extract 11 classes and more than 60 kinds of veterinary drug residues, such as sulfonamides, quinolones, macrolides, lincomycins, nitroimidazoles, beta-lactams, tetracyclines, chloromycetins, trinethoprims, chlordimeform, triadimenol and the like, the efficiency of analysis is high, and the detection cost is greatly reduced.

Description

technical field [0001] The invention relates to a method for simultaneous detection of multiple types of agricultural and veterinary drug residues in bee products, in particular to sulfonamides, quinolones, macrolides, lincosamides, nitroimidazoles, β-endo Simultaneous detection method for 11 major categories of pesticide and veterinary drug residues including amides, tetracyclines, chloramphenicol, sulfa synergists, chlordimeform, and triadimenol. Background technique [0002] At present, the detection of veterinary drug residues is still the main means of setting up technical barriers at home and abroad. Bee products and aquatic products are important animal-derived foreign exchange-earning products in my country, and are the focus of attention of developed countries such as the European Union. [0003] At present, domestic and foreign research on multi-residue analysis is mainly on pesticide residues. Pesticides are mostly water-insoluble nonpolar and weakly polar compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 徐锦忠丁涛吴斌沈崇钰彭涛陈惠兰张晓燕林宏蒋原陶宏锦
Owner 中华人民共和国江苏出入境检验检疫局
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