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Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry

A technology of ion mobility spectrometry and methyl bromide, which is applied in the field of fumigant methyl bromide residues, can solve the problems of high proficiency requirements for experimental operators, unstable recovery of analytes, and time-consuming detection methods, so as to reduce false positives and extract Good purification effect and reagent saving effect

Inactive Publication Date: 2015-10-28
ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0004] The detection of methyl bromide in food is now mostly carried out by gas chromatography. At present, there are few detection standards involving methyl bromide residues in food in China. Only the detection method for methyl bromide in grains promulgated by my country (SN 0649-1997. Residues of methyl bromide in grains for export Quantitative inspection method), the pretreatment method of this method uses an acid reflux extraction device to extract the sample, gas chromatography detection, the detection method is time-consuming, the consumption of reagents is large, the recovery of the analyte is unstable, and the proficiency of the experimental operators ask advanced questions

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  • Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry
  • Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry
  • Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry

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preparation example Construction

[0043] e) Preparation of standard solution: Accurately pipette the standard solution respectively, dissolve it in water and make a 2mg / mL stock solution, and dilute it into a standard working solution during use;

[0044] f) Use ion mobility spectrometry to detect standards and samples: the standard and samples are respectively drawn by the automatic headspace autosampler, injected into the ion mobility spectrometer, and after pre-separation by fast gas chromatography GC, the ions enter the ion in the form of a single component The IMS ionization area of ​​the migration spectrum reacts with the reagent ions produced by the ionization of the radioactive tritium source to form product ions; the product ions enter the IMS migration area under the action of ion pulses for two-dimensional separation; the separated ions finally reach the Faraday disk to complete qualitative and quantitative Detection, quantification by external standard method;

[0045] 4) Analysis of results

[00...

Embodiment 1

[0049] Methyl Bromide Detected in Rice Matrix

[0050] 1. Instruments and reagents

[0051] Instrument: Flavor Ion mobility spectrometry (Germany G.A.S company), equipped with a fully automatic headspace sampler; samples were injected through the headspace sampler, negative ion mode.

[0052] Reagents: saturated sodium chloride solution, methyl bromide standard solution 2000mg / L (purity not less than 95%, purchased from O2Si Company), and use water (secondary water) as solvent to prepare the required standard solution before use.

[0053] 2. Sample Processing

[0054] (1) Sample extraction: Accurately weigh 5.00±0.01g of the sample into a 20mL headspace sampling bottle, add 5mL of saturated sodium chloride solution, seal the cap, put it into the corresponding bottle position of the headspace sampler, and prepare Inject the sample to be tested.

[0055] (2) Standard working solution: add the corresponding standard solution into the sample bottle containing 5ml blank matrix...

Embodiment 2

[0061] The wheat sample was detected by gas chromatography electron capture detector (ECD), and methyl bromide was detected, and the sample was confirmed by ion mobility spectrometry.

[0062] Instruments and reagents

[0063] Instrument condition and pretreatment method are with embodiment 1

[0064] Results: Methyl bromide was not detected in the wheat samples.

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Abstract

The invention discloses a method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry. Bromomethane residues in a food sample are extracted by a saturated sodium chloride solution, a full-automatic headspace sample injection process is carried out and an ion mobility spectrometry-based detection process is carried out. A food matrix is pre-separated by rapid gas chromatography (GC), the separated food matrix in a single component form enters into an ion mobility spectrometry (IMS) ionizing zone and then reacts with reagent ions produced by radioactive tritium source ionization to produce product ions, the product ions enter into an IMS migration area under the action of ion pulse and are subjected to two-dimensional separation, and the separated ions are fed to a Faraday plate and are subjected to qualitative and quantitative detection, wherein an external standard method is used for quantification. The method has the characteristics of fastness, simpleness, high sensitivity, good separation effects, reagent saving and accurate and reliable qualitation and quantification and realizes separation of fumigation agent bromomethane residues in foods such as grains and fruits and fast qualitation and quantification.

Description

technical field [0001] The invention belongs to the technical field of food safety, and relates to a method for rapidly detecting residues of fumigant methyl bromide in food by using headspace sampling and ion mobility spectrometry. Background technique [0002] Methyl bromide, also known as methyl bromide or methyl bromide, is a colorless gas at normal temperature and pressure, usually odorless, but sweet in high concentrations. Molecular formula CH 3 -Br, molecular weight 94.95, relative density 1.730 (0-4°C), melting point -93.66°C, boiling point 3.6°C, has a strong fumigation effect, can kill various harmful organisms efficiently and broadly, and is often used in plant protection as a kill Insecticides, fungicides, soil fumigants and grain fumigants. However, as an insecticide that is invincible to harmful organisms, its toxicity to humans is also obvious: it is a strong nerve agent that can cause direct damage to human skin, lungs, kidneys, and liver. Severe poisonin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
Inventor 常春艳王利强陈旭艳葛含光王云凤葛宝坤
Owner ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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