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Method for detecting residual quantity of simazine in farmland environment based on gas chromatography-mass spectrometrometry

A technology for farmland environment and technology detection, applied in the field of detection of simazine residues in farmland environment, can solve the problems of complex pretreatment methods, inability to realize confirmatory analysis, early formulation time, etc.

Active Publication Date: 2018-02-02
沈阳海关技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the determination method was formulated earlier, compared with the current residue detection method, its pretreatment method is more complicated, the instrument is relatively backward, and it is impossible to realize the confirmation analysis

Method used

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  • Method for detecting residual quantity of simazine in farmland environment based on gas chromatography-mass spectrometrometry
  • Method for detecting residual quantity of simazine in farmland environment based on gas chromatography-mass spectrometrometry
  • Method for detecting residual quantity of simazine in farmland environment based on gas chromatography-mass spectrometrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] The present embodiment provides a method for detecting simazine residues in cow manure based on gas chromatography-mass spectrometry, which comprises the following steps:

[0097] Preparation of cow dung samples:

[0098] Take a representative sample of about 1 kg from all the cow dung samples, grind it through a homogenizer, and after mixing, divide it into two parts and put them into clean containers as samples. Seal and mark. In addition, during the sampling and sample preparation process, the samples should be prevented from being polluted or the residue content changes, and the obtained livestock and poultry feces samples should be stored frozen in an environment below -18°C.

[0099] Extract simazine from cow dung:

[0100] Add 50 mL of ethyl acetate-acetonitrile mixed solution with a volume ratio of 1:1 to 10.0 g of cow dung samples, homogeneously extract for 40 s, and centrifuge at a rate of 4000 r / min for 5 min to obtain extract A;

[0101] Use 10.0 g of anh...

Embodiment 2

[0131] The present embodiment provides a method for detecting simazine residues in soil based on gas chromatography-mass spectrometry, which comprises the following steps:

[0132] Soil sample preparation:

[0133] After the soil was collected, it was air-dried at room temperature to remove debris such as stones and grass roots, and then the air-dried soil was crushed, passed through a 100-mesh sieve, mixed thoroughly, and placed in a closed container for use.

[0134] In addition, during the operation of sampling and sample preparation, the samples should be prevented from being polluted or the residue content changes, and the obtained soil samples should be stored frozen in an environment below -18°C.

[0135] Extract simazine from soil:

[0136] Add 50 mL of acetonitrile to 10.0 g of soil sample, and ultrasonically extract at a rate of 4000 r / min for 30 min to obtain extract C; filter the extract C to obtain filtrate C and residue C;

[0137] Add 50 mL of acetonitrile to ...

Embodiment 3

[0159] This embodiment provides a method for detecting simazine residues in farmland irrigation water based on gas chromatography-mass spectrometry, which includes the following steps:

[0160] Preparation of farmland irrigation water samples:

[0161] Each collected water sample is at least 1L, and stored in an airtight container for later use. Shake well before measurement.

[0162] In addition, during the sampling and sample preparation process, the samples should be prevented from being polluted or the residue content changes, and the obtained farmland irrigation water samples should be stored frozen in an environment below -18°C.

[0163] Extraction of simazine in farmland irrigation water:

[0164] Add 2g of anhydrous sodium sulfate to 250mL of farmland irrigation water samples, dissolve evenly, use 50mL of methanol-acetonitrile mixed solution with a volume ratio of 1:4 to extract it, and collect the organic phase after standing for stratification;

[0165] Repeat the...

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Abstract

The invention provides a method for detecting the residual quantity of simazine in a farmland environment based on gas chromatography-mass spectrometrometry. The method comprises the following steps:1, extracting the simazine from a farmland environment sample to obtain a sample to be purified; 2, purifying the sample to be purified to obtain a sample to be detected; and 3, carrying out gas chromatography-mass spectrometrometry on the sample to be detected, and carrying out qualitative analysis and quantitative analysis on the simazine in the sample to complete the detection of the residual quantity of the simazine in the environment sample. The lowest detection limit of the detection method reaches 0.01 mg / kg, and the established detection method is simple, accurate and highly sensitive,and completely meets needs of the detection of the simazine in animal manure, soil, farmland irrigation water and other farmland environment samples.

Description

technical field [0001] The invention relates to a method for detecting simazine residues in farmland environment based on gas chromatography technology. Background technique [0002] Simazine is a highly selective systemic herbicide, molecular weight: 201.66; molecular formula: C 7 h 12 ClN 5 , CAS No.: 122-34-9, the structure is shown in the following formula: [0003] [0004] As a herbicide, simazine is widely used on corn, sorghum and other crops because of its high efficiency, low toxicity and specific selectivity, but its effective initial activity and residual activity can cause physiological changes in food animals. It interferes with the endocrine system, and at the same time has a moderate stimulating effect on the skin and respiratory tract, causing poisoning and causing great harm to humans, livestock and wild animals. [0005] Because simazine has toxic and side effects, the United States, Australia, Canada and other countries have set strict limits on th...

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 徐宜宏付海滨张敏赵颖钟钰
Owner 沈阳海关技术中心
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