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Method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS

A GC-NCI-MS, dibromochloropropane technology, applied in the field of pesticide residue detection, can solve the problems of cumbersome detection steps, large solvent consumption, poor reproducibility, etc., and achieves strong selectivity, good reproducibility and toxicity. small effect

Active Publication Date: 2015-12-02
广东中检达元检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The problem to be solved in the present invention is to provide a method for the determination of dibromochloropropane residues in fruits and vegetables by GC-NCI-MS for the above deficiencies, which overcomes the cumbersome detection steps of the traditional technology, the large amount of solvent and the benzene, ethane, concentrated sulfuric acid High toxicity, low sensitivity, low recovery, poor reproducibility, and the method is not suitable for the defects of fruit and vegetable substrates. The method of the present invention has the advantages of fast and simple detection, low toxicity, high sensitivity, strong selectivity, and good reproducibility. Advantages of high recovery rate

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  • Method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS
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  • Method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS

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Embodiment 1

[0026] Embodiment 1: take apple as example below, illustrate the assay method of dibromochloropropane residue, comprise the steps:

[0027] (1) Sample pretreatment

[0028] Weigh 15g of crushed and well-mixed apples, put them in a 100mL plastic centrifuge tube, add 15mL of 0.1% acetic acid / acetonitrile solution, 6.0g of anhydrous magnesium sulfate, and 1.5g of anhydrous sodium acetate, stir well with a glass rod, and place in Homogenize at high speed on a homogenizer for 2 minutes, 10000r / min, and centrifuge at 4°C for 10 minutes;

[0029] Take 10mL of the supernatant in a 250mL rotary evaporator, and evaporate until nearly dry, accurately add 2mL of acetonitrile to dissolve the residue, vortex mix at 1400r / min for 2min, transfer the solution into a centrifuge tube filled with 150mgPSA, 200mgC18 and 100ul toluene, 1400r / min Vortex for 2 minutes, purify the solution at 4000r / min, centrifuge for 10 minutes and filter with a 0.45um filter membrane for GC-NCI-MS analysis.

[003...

Embodiment 2

[0048] Embodiment 2, taking frozen spinach as an example, illustrates the assay method of dibromochloropropane residue, comprising the steps:

[0049] (1) Sample pretreatment

[0050] Weigh 15g of crushed and well-mixed frozen spinach, put it in a 100mL plastic centrifuge tube, add 15mL of 0.1% acetic acid / acetonitrile solution, 6.0g of anhydrous magnesium sulfate, and 1.5g of anhydrous sodium acetate, stir well with a glass rod, Homogenize on a homogenizer at high speed for 2min, 10000r / min, centrifuge at 4°C for 10min, take 10mL of the supernatant in a 250mL rotary evaporator, rotary evaporate until nearly dry, accurately add 2mL of acetonitrile to dissolve the residue, and vortex at 1400r / min for 2min , the solution was transferred into a centrifuge tube filled with 150mgPSA, 200mgC18 and 100uL toluene, and vortexed at 1400r / min for 2min. The purified solution was centrifuged at 4000r / min for 10min and then filtered with a 0.45um filter membrane for GC-NCI-MS analysis.

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Abstract

The invention discloses a method for measuring dibromochloropropane residues in fruits and vegetables by GC-NCI-MS. The method comprises the following steps: extraction, purification, preparation of a standard working solution and measurement by gas chromatography-negative chemical ionization-mass spectrometry, and combination of a dispersion solid phase extraction pretreatment technology and a GC-NCI-MS detection technology. The method is quick, simple and convenient; by virtue of utilizing acetic acid or acetonitrile as a solvent, the toxicity is low; the detection limit is as low as 0.75ug / kg, so the sensitivity is high; the recycling rate is 97.40-103.69 percent, so the selectivity is high; the RSD value is 3.02-5.74 percent, so the repetitiveness is high; interference of a matrix is effectively removed, and the method is suitable for detecting dibromochloropropane in various vegetables and fruits and products thereof; meanwhile, methylbenzene is added in the purification step of the dispersion solid phase extraction pretreatment technology, so that adsorption of purification powder PSA to a target is effectively reduced; in the same matrix, the recycling rate of the method is increased from 69.25-75.37 percent without methylbenzene to 97.96-10.3.69 percent.

Description

technical field [0001] The invention relates to a method for detecting the residual amount of dibromochloropropane, in particular to a method for qualitative and quantitative determination of dibromochloropropane in fruits and vegetables by gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) The method for residual amount belongs to the technical field of detection of pesticide residues. Background technique [0002] Dibromochloropropane, commonly known as black medicine, scientific name 1,2-dibromo-3-chloropropane, English name 1,2-Dibromo-3-chloropropane (abbreviation: DBCP), CAS number 96-12-8, molecular weight 236.3328 , the structural formula is: [0003] [0004] Dibromochloropropane is the active ingredient in liquid fumigant nematicides. It is a soil fumigant used in agriculture. It is suitable for the fumigation of seedbeds and greenhouses of vegetables, flowers, tobacco, strawberries and other crops to control root-knot nematodes, cys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 刘永强许文娟郭礼强孙军
Owner 广东中检达元检测技术有限公司
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