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GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix

A GC-NCI-MS, dibromochloropropane technology, applied in the field of pesticide residue detection, can solve the problems of low recovery rate, low sensitivity, large solvent consumption, etc., and achieves the removal of matrix interference, good reproducibility, and sensitivity. high effect

Active Publication Date: 2016-01-06
佛山市金城速冻食品有限公司
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  • 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 address the above deficiencies, and provide a GC-NCI-MS detection method for the residual amount of dibromochloropropane in a complex matrix for the first time, which overcomes the cumbersome detection steps, large solvent consumption, high toxicity, and low sensitivity of the traditional technology , low recovery rate, poor reproducibility, and the method is not suitable for the defects of complex matrices such as animal-derived foods. The method of the present invention has the advantages of fast and simple, small solvent consumption and low toxicity, high sensitivity, strong selectivity, and good reproducibility , suitable for the detection of dibromochloropropane in various animal-derived foods

Method used

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  • GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix
  • GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix
  • GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix

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Embodiment 1

[0027] Embodiment 1: take pork as an example below, illustrate the GC-NCI-M detection method of dibromochloropropane residual amount,

[0028] (1) Sample pretreatment

[0029] Weigh 10.00 g of the sample, place it in a 100 mL plastic centrifuge tube, add 40 mL of acetonitrile solution, homogenize at high speed for 1 min, then add 5 g of sodium chloride, homogenize at high speed for 1 min, and centrifuge at 4000 r / min for 5 min;

[0030] Take out 20mL of acetonitrile layer in a 250mL conical rotary evaporator, evaporate to near dryness on a rotary evaporator, add 3mL of acetonitrile-ethyl acetate mixed solvent with a volume ratio of 3:1 to dissolve the residue in the rotary evaporator, and wait for purification;

[0031] Install the ProElutCARB / NH2 cartridge on a solid-phase extraction device, add 2 g of anhydrous sodium sulfate to the cartridge, and then pre-wash the cartridge with 8 mL of acetonitrile-ethyl acetate mixed solvent with a volume ratio of 3:1 to keep The flow ra...

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Abstract

The invention discloses a GC-NCI-MS method for detection of dibromochloropropane residual quantity in complex matrix. The method is characterized by including the steps of extraction, purification, preparation of a standard working solution and gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) determination. The solid phase extraction technology and the gas phase chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) are combined to realize the qualitative identification and quantitative detection of dibromochloropropane in animal source foods. The method is quick and easy, uses ethyl acetate and acetonitrile as solvents, and has less toxicity. The method has detection limit as low as 0.98ug / kg, high sensitivity, recovery rate of 88.82-94.17%, strong selectivity, relative standard deviation of 2.48-3.77%, and good reproducibility, effectively removes the interference of the matrix, and is applicable to detection of dibromochloropropane in various in animal derived food.

Description

technical field [0001] The present invention relates to a method for detecting the residual amount of dibromochloropropane, more specifically, to a method for qualitatively and quantitatively measuring animal-derived foods and other complex matrices by gas chromatography-negative chemical source-mass spectrometry (GC-NCI-MS) The invention discloses a method for residual amount of dibromochloropropane in medium, belonging 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, tobacc...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N27/62
Inventor 刘永强许文娟孙军李凯
Owner 佛山市金城速冻食品有限公司
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