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Method for measuring residual quantity of ethyl 3-aminobenzoate in aquatic product

A technology of ethyl aminobenzoate and residues, which is applied in measuring devices, instruments, scientific instruments, etc., to achieve the effects of simple pretreatment, less interference, and solvent saving

Inactive Publication Date: 2015-11-04
CHINESE ACAD OF FISHERY SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for measuring the residual amount of ethyl aminobenzoate in aquatic products, which overcomes the disadvantages of complex pretreatment or purification of various solid-phase extraction columns in the existing method, and provides a mixed Solution extraction, QuEChERS reagent pack purification, after centrifugation, use HPLC-MS / MS equipped with an automatic sampler to directly determine the residual amount of ethyl aminobenzoate in aquatic products. This method has less interference, and the pretreatment is simple, fast, and efficient. Save solvent, accurate and sensitive

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: 1. Aquatic product sample preparation: Carp tissue is homogenized and stored in a -20°C refrigerator;

[0020] 2. Extraction: Melt surimi at room temperature, weigh 2g of sample into a 50mL centrifuge tube with a cover, add 10mL of mixed solution to fully infiltrate, vortex and mix well; add QuEChERS kit 1 (composed of 4g anhydrous magnesium sulfate, 1g chloride Sodium composition), immediately shake by hand to prevent the agglomeration of anhydrous magnesium sulfate, and centrifuge at 10000r / min for 10min;

[0021] 3. Purification: Pipette 1 mL of the sample extract supernatant into a 2 mL centrifuge tube, add QuEChERS kit 2 (composed of 300 mg N-propylethylenediamine bonded solid-phase adsorbent), vortex for 2 min, Centrifuge for 5 min at 1 / min, absorb the supernatant and filter it through a 0.22 μm organic phase filter membrane for HPLC-MS / MS analysis;

[0022] Instrument parameters: HPLC-MS / MS: with automatic sampler, capillary voltage 3.2kV; sheath g...

Embodiment 2

[0024] Embodiment two: dilute the ethyl aminobenzoate standard sample and be made into a series of mixed working solutions of 0.001~1mg / L with 7 grades of concentrations altogether, draw a standard curve with the concentration → ethyl aminobenzoate SRM ion peak area, obtain the correlation coefficient ( R 2 ); continuously reduce the injection concentration until the peak area is 3 times higher than the baseline noise as the limit of detection (LOD); respectively add 0.025, 0.05, 0.5mg / kg of three grades of concentration of ethyl aminobenzoate standard in the blank fish sample After extraction and purification, the sample was injected, the recovery rate was calculated, and repeated 3 times.

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Abstract

The invention discloses a method for measuring the residual quantity of ethyl 3-aminobenzoate in an aquatic product and relates to the technical field of physicochemical detecting of drug residues in aquatic products. An aquatic product sample is extracted through a mixed solution, purified through a QuEChERS reagent bag and centrifuged, and then the drug residual quantity in the aquatic product is measured through HPLC-MS / MS analysis. The method specifically comprises the following steps that preparing is conducted, wherein the fish body is dissected, subjected to homogenate and stored in a refrigerator at the low temperature of minus 20 DEG C; extracting is conducted; purifying is conducted, wherein liquid supernatant is sucked and filtered through 0.22 microns of organic phase filter membrane, and then the HPLC-MS / MS analysis is conducted. The method overcomes the defect that preprocessing is complex or a plurality of kinds of solid phases need to extract columellae for purification in an existing method, and mixed solution extracting is provided. According to the method, interferences are few, preprocessing is easy, convenient and quick, the solvent is saved, and accuracy and sensitivity are achieved.

Description

Technical field: [0001] The invention relates to the technical field of physical and chemical detection of drug residues in aquatic products, in particular to a method for measuring the residual amount of ethyl aminobenzoate in aquatic products. Background technique: [0002] my country is a big fishery country, and the total output of aquatic products has ranked first in the world for many years, which greatly meets people's demand for aquatic product consumption. However, high-density and large-scale farming also brings some negative effects, such as the pollution of the water environment, and various drug residues in aquatic products exceed the standard. Drugs in aquatic products will accumulate and concentrate in organisms through the food chain and eventually be delivered to the human body, which poses a potential hazard to human food safety. The trade name of ethyl m-aminobenzoate is fish diazepam, which often exists in the form of ethyl m-aminobenzoate methanesulfona...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 李晋成刘欢宋怿
Owner CHINESE ACAD OF FISHERY SCI
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