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Method for determining diuron residues in sugarcane based on 3,4-dichloroaniline

A technology of dichloroaniline and diuron, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the difficulties in meeting the requirements of fast, low-cost, environmental protection detection, gas chromatography and quantitative analysis, and the consumption of mobile phase reagents Large volume and other problems, to achieve the effect of symmetrical peak shape, uniform distribution, and low matrix effect

Active Publication Date: 2018-11-16
GUANGXI NORMAL UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Diuron decomposes when the temperature reaches above 180°C, which brings difficulties to gas chromatography and quantitative analysis. Most studies use liquid chromatography for analysis, but when liquid chromatography-mass spectrometry is used, the detection cost is high It is difficult to meet the requirements of rapid, low-cost and environmental protection detection due to the large consumption of mobile phase reagents

Method used

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  • Method for determining diuron residues in sugarcane based on 3,4-dichloroaniline
  • Method for determining diuron residues in sugarcane based on 3,4-dichloroaniline
  • Method for determining diuron residues in sugarcane based on 3,4-dichloroaniline

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Experimental program
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Embodiment 1

[0037] The method for determining the indicator components of diuron thermal decomposition in the gas chromatography-electron capture detector method is as follows:

[0038] (1) Establishment of gas chromatography conditions: column model: HP-5MS; column specification: 30 m × 250 μm × 0.25 μm; carrier gas is helium with a purity greater than 99.999%; carrier gas flow rate is 1.2 mL / min; The temperature of the sample port is 250°C, the temperature of the detector is 300°C, and the temperature of the column oven is programmed. ℃, hold for 2 min; injection volume: 1L, split ratio: 1:5; establishment of mass spectrometry conditions: ion source: electron bombardment source; electron energy: 70eV; gas chromatography-mass spectrometry interface temperature: 250°C; quadrupole Temperature: 150°C; ion source temperature: 230°C, acquisition mode: selected ion monitoring SIM, 3,4-dichloroaniline quantified ion is m / z 161 ion, qualitative ion is m / z 161, 207, 126, 63 ions;

[0039] (2) A...

Embodiment 2

[0043] On the basis of embodiment 1, measure the method for diuron residual in sugarcane, comprise the steps:

[0044] S1. Sample pretreatment: extract and purify the sugarcane sample to obtain the sugarcane solution to be tested;

[0045] S2. Prepare 7 concentrations of diuron standard solutions (0.01, 0.05, 0.1, 0.5, 1.0, 2.0, and 5.0 mg / L); perform gas chromatography-electron capture detection on the prepared diuron standard solutions of each concentration gradient Determination of the instrument, the chromatographic peak area of ​​the standard solution is used for regression analysis of its corresponding concentration, and the standard working curve is drawn; under the same conditions, the sugarcane test solution is injected into the gas chromatography-electron capture detector for measurement, and the sugarcane test solution is measured. The chromatographic peak area of ​​diuron was substituted into the standard working curve to obtain the content of diuron in the sugarca...

Embodiment 3

[0050] Precision and spike recovery experiments

[0051] Sugarcane juice without diuron was used as a blank sample, and each sample was subjected to recovery experiments at the levels of 0.01 mg / kg, 0.05 mg / kg, and 0.5 mg / kg, and 6 parallel samples were made for each level of addition. Measure according to the method in embodiment 2, ask its average recovery rate and relative standard deviation.

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Abstract

The invention discloses a method for determining diuron residues in sugarcane based on 3,4-dichloroaniline. The method comprises the following steps: S1) employing a gas chromatography-mass spectrometry to determine an indication component 3,4-dichloroaniline for diuron thermal decomposition; S2) sample pre-processing: extracting a sugarcane sample and purifying the sugarcane sample to obtain sugarcane to-be-detected liquid; and S3) preparing at least 6 diuron standard solutions with different concentrations, performing gas chromatography-electron capture detector determination on the diuron standard solutions with concentration gradients, drafting a standard work curve, and determining the content of diuron in the sugarcane to-be-detected liquid. According to the method, diuron has good linear relation in a scope of 0.01-5.0 mg / L, the correlation coefficient is greater than 0.998, the detection limit is 0.007 mg / kg, the recovery rate of diuron in the sugarcane juice is 89.2%-111%, andthe relative standard deviation is 2.45-6.57%. The accuracy and precision of the method can satisfy the residual analysis requirement of pesticide.

Description

technical field [0001] The invention relates to the technical field of food safety, in particular to a method for determining residues of diuron in sugarcane based on 3,4-dichloroaniline. Background technique [0002] Diuron (Diuron) is a substituted urea herbicide, which can effectively control grass weeds, broad-leaved weeds and algae. Since the efficacy of this herbicide is not limited by geographical and climatic conditions, it is widely used throughout the country. Applied in sugarcane, corn, soybean and other crop fields, due to its stable chemical properties and long residual period, Diuron persists in the environment and has a certain bioaccumulation effect, which is harmful to mammals, birds, fetal development and human health. Toxic effects, according to the "National Food Safety Standard Sugar GB13104-2014" promulgated and implemented on May 24, 2015, the original hygiene standard was upgraded to the national food safety standard, and food additives and pollutants...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 王小明陈碧廖政达谢济运孙晓波
Owner GUANGXI NORMAL UNIV OF SCI & TECH
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