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Detection method for extracting albendazole compounds from fish flesh

A technology of albendazole and detection method, which is applied in the field of environmental protection, can solve problems such as high cost, increased detection cost, and lack of good matching regulations, and achieve the effect of simplifying pretreatment steps and reducing detection cost

Inactive Publication Date: 2018-11-16
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solid phase extraction is complex and expensive
The introduction of internal standards, especially isotope internal standards, increases the cost of detection and is not conducive to popularization
Most of the literature does not match the regulations of relevant national institutions or international organizations on the MRL of albendazole when testing dozens or even hundreds of veterinary drugs at the same time

Method used

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  • Detection method for extracting albendazole compounds from fish flesh
  • Detection method for extracting albendazole compounds from fish flesh
  • Detection method for extracting albendazole compounds from fish flesh

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A detection method for extracting albendazole compounds from fish meat. It is found that ethyl acetate, a commonly used extractant for extracting benzimidazoles from a high-protein matrix, has impurities that can quickly oxidize ABZ to ABZ-SO, including the following steps:

[0043] (1) Preparation of sample a

[0044] Take 7.5mL ethyl acetate into a 15mL polypropylene centrifuge tube, blow nitrogen at room temperature to dryness, add 1mL500μg / L mixed standard working solution (containing ABZ, ABZ-SO, ABZ-SO 2 And ABZ-NH 2 -SO 2 , The solvent is 20% methanol aqueous solution), vortex for 1 min, pass through a 0.45 μm organic phase needle filter, and then detect with high performance liquid chromatography (ultraviolet detector).

[0045] (2) Preparation of sample b

[0046] Take 30mL of ethyl acetate from the same reagent bottle and put it in a 100mL rotary steaming bottle, and then evaporate to dryness under reduced pressure at 40℃. Take 7.5mL from the collected fraction and put...

Embodiment 2

[0060] A detection method for extracting albendazole compounds from fish meat, screening qualified ethyl acetate, selecting ethyl acetate from different manufacturers (2 bottles of Merck chromatographic purity, 2 bottles of Sigma-Aldrich chromatographic purity, 1 bottle of Shandong Fuyu Chemical Analytical purity, one bottle of Merck and one bottle of Sigma-Aldrich chromatographic pure ethyl acetate were confirmed to be fresh enough), and the processing steps are the same as the preparation of sample a in Example 1. At the same time, prepare a standard solution, and the processing steps are consistent with the preparation of sample c in Example 1. The HPLC conditions are the same as in Example 1. See the survey results image 3 .

[0061] From image 3 The results show that there are no impurities in the fresh ethyl acetate of Sigma-Aldrich and Merck that can quickly oxidize ABZ to ABZ-SO. The old ethyl acetate of Merck has deteriorated significantly, and it is compared with the...

Embodiment 3

[0063] A detection method for extracting albendazole compounds from fish meat, investigating the influence of the commonly used degreasing solvent n-hexane on the recovery rate of albendazole, including the following steps:

[0064] (1) Preparation of sample a

[0065] Take 1mL 500μg / L mixed standard working solution (containing ABZ, ABZ-SO, ABZ-SO 2 And ABZ-NH 2 -SO 2 , The solvent is 20% methanol aqueous solution) into a 4mL polypropylene centrifuge tube, then add 1mL n-hexane, vortex for 1min, and centrifuge at 6000rpm for 5min. Transfer the upper layer of n-hexane to a new 4mL polypropylene centrifuge tube. Add 1 mL of n-hexane to the lower aqueous solution, vortex for 1 min, and centrifuge at 6000 rpm for 5 min. The upper layer of n-hexane was combined into the second centrifuge tube, nitrogen was blown to dryness at room temperature, 1 mL of 20% methanol aqueous solution was added, vortexed for 1 min, passed through a 0.45 μm organic phase needle filter, and then detected by...

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Abstract

The invention discloses a detection method for extracting albendazole compounds from fish flesh. The method comprises the following steps: extraction of homogenized fish flesh with ethyl acetate, purification using n-hexane, acetonitrile concentrating, external standard technology quantification and high performance liquid chromatography-tandem mass spectrometry detection. A technology for rapidlyscreening qualified ethyl acetate is provided to avoid possible impurities which can oxidize albendazole. The detection limits of albendazole sulfoxide, albendazole sulfone and amino albendazole sulfone in the method are 0.27 [mu]g / kg, 0.09 [mu]g / kg and 0.11 [mu]g / kg respectively. The maximum residue limit of albendazole in ruminants in European Union and China is prescribed as follows: the sum of residual markers albendazole sulfoxide, albendazole sulfone and amino albendazole sulfone in a muscle matrix does not exceed 100 [mu]g / Kg. The method is very suitable for detecting the residue of albendazole in the fish flesh, and has the advantages of simplicity, fastness, low cost and high sensitivity.

Description

[0001] The invention relates to a detection method for extracting albendazole compounds from fish meat, and belongs to the technical field of environmental protection. Background technique [0002] Albendazole (ABZ) is a highly effective and broad-spectrum anthelmintic, which is widely used in many fields including aquaculture. In organisms, albendazole is rapidly metabolized into three main metabolites: albendazole sulfoxide (ABZ-SO), albendazole sulfone (ABZ-SO) 2 ) And albendazole aminosulfone (ABZ-NH 2 -SO 2 ). Its anthelmintic activity is mainly determined by its primary metabolite ABZ-SO, which can also be used as an anthelmintic alone. Animal experiments have found that both ABZ and ABZ-SO have teratogenic effects. It is proposed in the literature that in the initial stage after taking ABZ, the most likely residues to be detected in the organism are ABZ-SO and ABZ-SO 2 , The longest remaining time is ABZ-NH2-SO 2 . At present, the definition of the maximum residue limit ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 宋相志张燕飞苏远安
Owner CENT SOUTH UNIV
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