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Pretreatment method and quantitative analysis method for rapid determination of abamectin pesticide residues in edible oil

A technology of abamectins and pesticide residues, which is applied in the direction of measuring devices, analysis materials, material separation, etc., can solve the problems of high-throughput detection of unfavorable samples, consume a large amount of organic solvent, and consume a lot of time, so as to avoid surface Modification process, good effect, fast pretreatment effect

Active Publication Date: 2019-04-09
厦门鹭珈聚芯生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The pretreatment method for the detection of pesticide residues in edible oil generally includes two important steps: the extraction of the target analyte from the sample and the purification of the extract, which is usually extracted by liquid-liquid extraction, and the extract is separated by centrifugation or standing still. After layering, the upper organic phase is taken for the next step of purification operation. This process consumes a large amount of organic solvents and has many steps, which is not conducive to the high-throughput detection of a large number of samples.
For example: when Huang et al. analyzed ABA and IVM in edible oil, they used liquid-liquid extraction (LLE) and low-temperature precipitation purification methods to remove co-extraction interference substances. Extraction of similar substances makes the method involve a multi-step extraction and purification process, and the freezing process takes a lot of time and is time-consuming and labor-intensive

Method used

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  • Pretreatment method and quantitative analysis method for rapid determination of abamectin pesticide residues in edible oil
  • Pretreatment method and quantitative analysis method for rapid determination of abamectin pesticide residues in edible oil
  • Pretreatment method and quantitative analysis method for rapid determination of abamectin pesticide residues in edible oil

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Experimental program
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Effect test

Embodiment 1

[0038] A pretreatment method for the rapid determination of abamectin pesticide residues in edible oil, such as figure 1 As shown, the steps are as follows:

[0039] 1) Weigh 0.1g edible oil sample into a 4mL centrifuge tube, dissolve and dilute the above-mentioned edible oil sample to be tested with 1mL n-hexane, vortex for 1min, add 30mg Fe 3 O 4 As the adsorbent for magnetic solid phase extraction, after vortex extraction for 1 min, separate the adsorbent from the solution under the action of an external magnetic field, and discard the supernatant;

[0040] 2) Wash the adsorbent obtained in step 1) with 1 mL of n-hexane-ethyl acetate (80 / 20, v / v) for 1 min, then desorb with 1 mL of methanol, and use N 2 After drying, use 0.2mL acetonitrile-water (90 / 10, v / v) to reconstitute, the resulting solution is the test solution for the rapid determination of avermectin pesticide residues in edible oil, and the subsequent LC-MS / MS Analysis is a rapid detection method for the determination o...

Embodiment 2

[0046] In order to verify the feasibility of the detection method for rapid determination of abamectin pesticide residues in edible oil provided by the present invention in practical applications, the linearity, limit of detection (LODs), limit of quantification (LOQs), Parameters such as precision were investigated. In the LC-MS / MS analysis, the matrix effect will seriously affect the results of the analyte quantitative analysis. In order to avoid the matrix effect, a blank matrix matching calibration curve is used in this embodiment. The process of establishing the calibration curve is as follows:

[0047] 1) Weigh 0.1g blank edible oil sample into a 4mL centrifuge tube, dissolve the diluted oil sample with 1mL n-hexane, and vortex for 1min, then add 30mg Fe 3 O 4 As the adsorbent for MSPE, after vortex extraction for 1 min, the adsorbent and the solution are separated under the action of an external magnetic field, and the supernatant is discarded; the obtained adsorbent is 1m...

Embodiment 3

[0053] In order to evaluate the accuracy of the detection method for rapid determination of avermectin pesticide residues in edible oil provided by the present invention, the recovery rate of the method was investigated in this example. Specific steps are as follows:

[0054] 1) Weigh 0.1g blank edible oil sample and place it in a 4mL centrifuge tube, add low (10μg / kg), medium (50μg / kg), high (200μg / kg) target analyte (i.e. Bacteriocin pesticide), after standing for 30 min, dissolve the diluted oil sample with 1 mL of n-hexane, vortex for 1 min, and add 30 mg Fe 3 O 4 As the adsorbent for magnetic solid phase extraction, after vortex extraction for 1 min, the adsorbent is separated from the solution under the action of an external magnetic field, and the supernatant is discarded; the obtained adsorbent uses 1 mL n-hexane-ethyl acetate (80 / 20, v / v) After washing for 1 min, 1 mL of methanol is desorbed; the methanol in the obtained desorption solution is desorbed with N 2 After dry...

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Abstract

The invention discloses a pretreatment method for rapidly determining residues of abamectin pesticide in edible oil, and a quantitative analysis method thereof. The pretreatment method comprises the following steps: (1) diluting the edible oil, adding magnetic ferroferric oxide microspheres to perform magnetic solid phase extraction on the abamectin pesticide in the edible oil; (2) after the extraction is completed in step (1), separating solids from liquid, wherein an obtained solid product is magnetic ferroferric oxide microspheres absorbing the abamectin pesticide residue, washing, desorbing, and re-dissolving the magnetic ferroferric oxide microspheres, wherein an obtained solution is a solution to be determined for rapidly determining the residue of the abamectin pesticide in the edible oil; and (3) performing the quantitative analysis by adopting an external standard method by virtue of liquid phase chromatography-tandem mass spectrum. The pretreatment process of the invention can remove a great number of matrixes in the edible oil, is good in purification effect, good in recovery of pesticide, capable of greatly increasing the separation efficiency of the pesticide by combining the liquid phase chromatography and the tandem mass spectrum, is high in detection sensitivity and accuracy and good in reproducibility.

Description

Technical field [0001] The invention belongs to the technical field of rapid analysis and detection, and particularly relates to a pretreatment method and a quantitative analysis method for quickly determining the residue of abamectin pesticides in edible oil. Background technique [0002] Abamectins are insecticides with macrolide structure and are widely used in agriculture and livestock production. In my country, the most commonly used abamectins are mainly abamectin (ABA), emamectin (EMA) benzoate and ivermectin (IVM). ABA is produced by the fermentation of Streptomyces avermitilis in actinomycetes, and is the precursor of EMA benzoate and IVM. EMA benzoate and IVM modify the disaccharide at the ABA end and reduce C, respectively 22 , C 23 Unsaturated double bonds between positions are obtained. However, scientists have confirmed through animal experiments: Abamectin drugs are toxic to mammals including humans. Although they will not cause genetic mutations and cancer, they...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 彭西甜鲁维张惠贤周有祥夏虹胡西洲王小飞夏珍珍张仙刘丽彭茂民彭立军
Owner 厦门鹭珈聚芯生物科技有限公司
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