Method for determining residue of emamectin benzoate in aquatic product material

A method of determination, the technology of inmetine, applied in material separation, analysis of materials, measuring devices, etc., can solve the problem of technical support for the maximum residue limit of inmetine, lack of detection methods, and no literature reports on any relevant detection methods, etc. problem, to achieve the effect of optimizing the purification treatment steps and conditions, simple sample treatment operation, and easy operation

Active Publication Date: 2018-12-11
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Since the Codex Alimentarius Commission (CAC) newly increased the maximum residue limit of emetine in 2015, there is no standard for the detection of emetine residues in aquatic products, and there is no literature report on any relevant detection methods. It is difficult to provide technical support for the relevant regulatory authorities in my country to formulate the maximum residue limit of phenmettin in the detection method of phenmettin. The method of the present invention is to detect the residual amount of phenmettin in aquatic products. The method adopts ethyl acetate as the extraction solution. , using a mixed cation-exchange solid-phase extraction column for purification, using a Waters Atlantis T3 (4.6mm×100mm, particle size 3μm) chromatographic column for separation, using acetonitrile-5mM formic acid aqueous solution as the mobile phase, gradient elution, and selecting a qualitative ion pair: 886.5> 158.3, collision energy 121V; 886.5>81.9, collision energy 42V; 886.5>158.3 with less interference is selected as the quantitative ion pair, and quantified by external standard method

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  • Method for determining residue of emamectin benzoate in aquatic product material
  • Method for determining residue of emamectin benzoate in aquatic product material
  • Method for determining residue of emamectin benzoate in aquatic product material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1: Detection of Enmetine in Tilapia and Shrimp

[0057] 1. Reagents

[0058] All reagents used were of analytical grade unless otherwise specified. Water is first-class water in accordance with GB / T 6682; Inmetine standard: content ≥ 98%; acetonitrile: chromatographically pure; ethyl acetate: chromatographically pure; formic acid: chromatographically pure.

[0059] 5mM formic acid aqueous solution: Take 192μL of formic acid, dissolve in water and dilute to 1000mL.

[0060] Fixed solution: Take 25mL of acetonitrile and 75mL of 2% formic acid aqueous solution, mix well, set aside.

[0061] Mobile phase solution: Take 50mL of acetonitrile and 50mL of 5mM formic acid aqueous solution, mix well, and set aside.

[0062] 100 μg / mL Inemetine standard stock solution: Accurately weigh 10 mg of Inmetine standard substance, dissolve it in acetonitrile and dilute to the mark in a 100 mL measuring bottle, and prepare the Inmetine standard stock solution with a concentratio...

Embodiment 2

[0117] Embodiment 2: Sensitivity, accuracy and precision test

[0118] 1 Sensitivity test

[0119] 1.1 Determination of quantitation limit

[0120] The limit of quantitation was determined based on the value of the signal-to-noise (S / N) ratio. Add 0.5 μg / kg of inmetine standard solution to blank tilapia and shrimp respectively, and measure the ratio of signal to noise. When S / N≥10 and the recovery rate and relative standard deviation meet the requirements of the residue detection method concentration is the limit of quantitation. Experimental results: The quantitative limit of this method is 0.5μg / kg.

[0121] 1.2 Accuracy test

[0122] Accurately weigh 5.0g of blank sample into a 50mL centrifuge tube, add a series of standard working solutions of known concentration to prepare tissue samples containing einastatin at concentrations of 0.5, 1.0, and 5.0 μg / kg, and do 6 parallels were measured according to the sample pretreatment process, and the recovery rate of the standa...

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Abstract

The invention discloses a method for determining the residue of emamectin benzoate in an aquatic product material and application. The method specifically comprises the steps that a sample is directlyground and homogenized, ethyl acetate is adopted to serve as an extraction solvent, after part of extraction liquid is concentrated to a constant volume, the extraction liquid is purified through a solid-phase extraction column, a liquid chromatogram-tandem mass spectrometer is utilized for detecting, and quantification is conducted by using an external standard method. The invention firstly provides a standard method for detecting the residue of emamectin benzoate in the aquatic product material, and fills up the technical blank of the field. The related coefficient of the regression equation reaches 0.99 or above, the testing minimum is 0.5 microgram/kg, the recycling rate at the 0.5 microgram/kg-5.0 microgram/kg fortified concentration level is 80%-120%. The relative standard deviationin a laboratory is less than or equal to 20%. The method is easy and convenient to operate, the sensitivity is high, the interference resistance is high, qualitative and quantitative operation is conducted scientifically and accurately, and technical support can be provided for related supervision departments in China to make the maximum residue limit of emamectin benzoate in aquatic products.

Description

technical field [0001] The invention relates to the technical field of detection of veterinary drug residues, and more specifically relates to a method for determining the residues of enmetine in aquatic product materials, especially tilapia, shrimp or crab. Background technique [0002] Veterinary drug residues in aquatic products directly affect human health. [0003] Emamectin, also known as Emamectin, has the molecular formula C 49 h 75 NO 13 , the molecular weight is 886.51, and its structural formula is as shown in formula (I): [0004] [0005] Emamectin is a new type of high-efficiency, broad-spectrum anthelmintic. The Codex Alimentarius Commission (CAC) increased the maximum residue limit of emetine in 2015, allowing it to be used in aquatic products and setting the maximum residue limit: 100 μg / kg in salmon and trout muscle. Japan's positive list also stipulates that the maximum residue limit in aquatic animals such as fish fillets, crabs, and frozen shrimp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/88G01N30/54
CPCG01N30/02G01N30/54G01N30/88G01N2030/884G01N2030/027
Inventor 欧阳少伦林峰蓝草邵琳智吴映璇姚仰勋邹游
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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