Pretreatment method for rapidly determining residues of abamectin pesticide in edible oil, and quantitative analysis method

A technology for abamectins and pesticide residues, which is applied in measurement devices, analytical materials, material separation, etc., can solve problems such as high-throughput detection of unfavorable samples, consumption of large organic solvents, consumption of large amounts of time, etc., to avoid surface Modification process, good effect, fast pretreatment effect

Active Publication Date: 2017-06-23
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 for rapidly determining residues of abamectin pesticide in edible oil, and quantitative analysis method
  • Pretreatment method for rapidly determining residues of abamectin pesticide in edible oil, and quantitative analysis method
  • Pretreatment method for rapidly determining residues of abamectin pesticide in edible oil, and quantitative analysis method

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Experimental program
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Effect test

Embodiment 1

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

[0039] 1) Weigh 0.1g edible oil sample and place it in a 4mL centrifuge tube, dissolve and dilute the above edible oil sample to be tested with 1mL n-hexane, vortex for 1min, add 30mg Fe 3 o 4 As an adsorbent for magnetic solid-phase extraction, after vortex extraction for 1 min, the adsorbent and the solution were separated under the action of an external magnetic field, and the supernatant was discarded;

[0040] 2) Wash the adsorbent obtained in step 1) with 1 mL of n-hexane-ethyl acetate (80 / 20, v / v) for 1 min, desorb with 1 mL of methanol, and desorb the obtained desorption solution with N 2 After drying, redissolve with 0.2mL acetonitrile-water (90 / 10, v / v), and the resulting solution is the test solution for rapid determination of abamectin pesticide residues in edible oil, and the subsequent LC-MS / MS Analy...

Embodiment 2

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

[0047] 1) Weigh 0.1g of a blank edible oil sample and place it in a 4mL centrifuge tube, dissolve and dilute the oil sample with 1mL of n-hexane, and vortex for 1min, then add 30mg of Fe 3 o 4 As an adsorbent for MSPE, after vortex extraction for 1 min, the adsorbent and the solution were separated under the action of an external magnetic field, and the supernatant...

Embodiment 3

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

[0054] 1) Weigh 0.1g of blank edible oil sample and place it in a 4mL centrifuge tube, add low (10μg / kg), medium (50μg / kg) and high (200μg / kg) target analytes (i.e. avi Bacterin pesticide), after standing for 30min, dissolve the diluted oil sample with 1mL n-hexane, and vortex for 1min, add 30mg Fe 3 o 4 As an adsorbent for magnetic solid-phase extraction, after vortex extraction for 1 min, the adsorbent and the solution were separated under the action of an external magnetic field, and the supernatant was discarded; the obtained adsorbent was washed with 1 mL of n-hexane-ethyl acetate (80 / 20, v / v) After washing for 1 min, 1 mL of methanol was desorbed; 2 After drying, add 0.2mL of acetonitrile-water (90 / 10,...

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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, in particular to a pretreatment method and a quantitative analysis method for rapid determination of avermectin pesticide residues in edible oil. Background technique [0002] Abamectins are insecticides with a macrolide structure and are widely used in agriculture and livestock production. In my country, the most commonly used avermectins are mainly abamectin (ABA), emamectin emamectin (EMA) benzoate and ivermectin (IVM). ABA is produced by fermentation of the actinomycete Streptomyces avermitilis and is the precursor of EMA benzoate and IVM. EMA benzoate and IVM modify the disaccharide at the end of ABA and reduce the C 22 、C 23 The unsaturated double bond between the positions is obtained. However, scientists have confirmed through animal experiments that avermectins have certain toxicity to mammals including humans. Although they do not cause gene mutations and cancer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
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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