Method for determining residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food

A plant-derived technology of methyl isothiocyanate, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of manpower and material resources, cost, unfavorable daily promotion and use, etc., and achieve the effect of simple operation and low cost

Pending Publication Date: 2022-04-22
厦门海关技术中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the existing relevant literatures, the detection methods of damaron and its metabolite methyl isothiocyanate all use different pretreatment methods and different instruments and equipment to detect damaron and methyl isothiocyanate respectively, such as Feng Yizhi et al. Use liquid chromatography to determine the cotton wool in tomato and soil, and use gas chromatography-mass spectrometry to measure methyl isothiocyanate in tomato and soil. Two pretreatment method

Method used

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  • Method for determining residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food
  • Method for determining residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food
  • Method for determining residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food

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Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1 determines analytical instrument

[0036] According to the methods established by Feng Yizhi, Xu Feng, etc., it can be known that liquid chromatography, ultra-high performance liquid chromatography-tandem mass spectrometry can be used to analyze dasyron, and gas chromatography or gas chromatography can be used to analyze methyl isothiocyanate. The present invention aims to establish and use the same pretreatment method and instrument method to detect and confirm datamone and methyl isothiocyanate, and to abandon the use of gas chromatograph and liquid chromatograph when selecting detection instruments, and only choose to try qualitative More capable ultra-high performance liquid chromatography-tandem mass spectrometer, GC-MS and triple quadrupole GC-MS. Firstly, according to the method development procedure of ultra-high performance liquid chromatography-tandem mass spectrometer, the parent ion scanning and product ion scanning of damannon and methyl isothi...

Embodiment 2

[0037] Embodiment 2 determines chromatographic column

[0038] It can be seen from the literature that the analysis of methyl isothiocyanate in the article of Xu Feng et al. uses DB-1 (30m, 0.25mm, 0.25μm), and the stationary phase of this chromatographic column is 100% dimethyl polysiloxane, which is non-polar The article of Feng Yizhi et al. used TG-1701MS (30m, 0.25mm, 0.25μm) to analyze methyl isothiocyanate, and the stationary phase of this column was 14% cyanopropylphenyl / 86% di Polysiloxane, medium polarity, low bleed column. Therefore, methyl isothiocyanate can be analyzed using non-polar and medium polar columns.

[0039] Exploratory experiments compared DB-5MS, DB-17MS, and DB-1701 three chromatographic columns, wherein the stationary phase of DB-5MS is (5%-phenyl)-methylpolysiloxane, which is a non-polar chromatographic column. The polarity is equivalent to that of DB-1 column; the stationary phase of DB-17MS is (50%-phenyl)-methyl polysiloxane, with medium polari...

Embodiment 3

[0041] Embodiment 3 determines the injection temperature

[0042] In the existing literature, when gas chromatography is used to detect methyl isothiocyanate, the inlet temperature is 150°C, the detector temperature is 200°C, the gas interface temperature is 180°C, and the relevant temperature settings are all relatively low. The experiment compares the different operating conditions of the inlet temperature of 150°C, the gas interface temperature of 180°C, and the ion source temperature of 200°C, and the inlet temperature of 280°C, the gas interface temperature of 280°C, and the ion source temperature of 230°C. The difference between the response of methyl cyanate and danoron, as a result, the response difference of the two substances at different instrument temperatures is within 5%, that is, the two substances will not be unstable because of high temperature, so the present invention finally selects the instrument temperature setting For: the inlet temperature is 280°C, the...

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Abstract

The invention relates to a method for measuring the residual quantity of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food, which comprises the following steps: pretreatment: crushing a sample to be measured, adding ethyl acetate, performing vortex oscillation for extraction, and then centrifuging; sucking the supernate, adding ethylenediamine-N-propyl silanized silica gel, graphitized carbon black, C18 and anhydrous magnesium sulfate for purification, carrying out vortex mixing, centrifuging, taking the supernate, and filtering a membrane to obtain an extracting solution; detecting the extracting solution by a gas chromatography-triple quadrupole mass spectrometer, and quantifying by a matrix matching external standard method. According to the method, the linear relation of the target compound in the range of 0.01-0.10 mg/kg is good, and correlation coefficients are all larger than 0.99. The average recovery rate of a blank sample at low, medium and high addition levels is 81.5%-109.4%, the relative standard deviation (n = 6) is 2.8%-9.0%, and the limit of quantitation of the method is 0.01 mg/kg. The method is simple, rapid and sensitive to operate, and can meet the detection requirements of dazomet and metabolite methyl isothiocyanate thereof in plant-derived food.

Description

technical field [0001] The invention relates to a detection technology for pesticide residues, in particular to a method for determining the residues of dacetamone and its metabolite methyl isothiocyanate in plant-derived foods. Background technique [0002] Dipyron, the chemical name is 3,5-dimethyl-1,3,5-thiadiazine-2-thione, is a stable crystalline solid at room temperature, has a fumigation effect, and is often used to control soil fungi, kill It can effectively kill root-knot nematodes, soil pests, weeds and various soil-borne diseases, so as to obtain clean and healthy soil; it is an ideal soil treatment agent to replace methyl bromide. In acidic soils, it slowly decomposes to release methyl isothiocyanate, methylamine, carbon disulfide and hydrogen sulfide, which diffuse upward through spaces in the soil, killing organisms that come into contact with it. When agricultural products are planted in the soil treated with cotton wool, residues in food will be caused, whic...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/72G01N30/8679G01N2030/047
Inventor 荣杰峰徐敦明许美珠邹强张志勇
Owner 厦门海关技术中心
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