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Analysis and detection method for glyphosate in domestic drinking water

A detection method, glyphosate-medium technology, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve problems such as short running time, affecting quantitative accuracy, and non-detection, so as to save time and labor, and save manpower and time, the effect of simple and easy operation

Inactive Publication Date: 2019-08-30
北京市水文总站
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chromatographic conditions used are: EGC (KOH) eluent online generator automatically generates 30mmol KOH eluent online, isocratic eluting at a flow rate of 1.20mL / min, 25μL injection volume, inhibition conductivity detection, 90mA inhibition current, column The temperature of the box is 25°C, the temperature of the detection cell is 35°C, and the chromatographic run time is 10 minutes. It has the following disadvantages: 1) the flow rate is fast, which will cause the pressure of the instrument to increase, the baseline stability to deteriorate, and the noise to increase; The sample volume is too small: it will cause inaccurate or even undetectable quantification of low-level target substances to be tested, and there will be deviations in the test results. Small sample volumes also have relatively high requirements for the accuracy of the analytical column, suppressor, and conductivity detector of the instrument , which is not conducive to the promotion and application of the method; 3) The running time is short: it affects the separation effect of each component in the sample, especially when there are many types of ions in the sample to be tested or the content of some components is too large, it will be treated as The measured components cause shadowing and affect the accuracy of quantification

Method used

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  • Analysis and detection method for glyphosate in domestic drinking water
  • Analysis and detection method for glyphosate in domestic drinking water
  • Analysis and detection method for glyphosate in domestic drinking water

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Experimental program
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Effect test

Embodiment 1-1

[0081] The analytical detection method of glyphosate in the determination sample of embodiment 1-1

[0082] (1) Determine the operating parameters of the ion chromatograph: the eluent is 30mmol / L potassium hydroxide solution, the mobile phase flow rate: 1.0mL / min, the injection volume: 100μL, the conductivity cell temperature: 30.0°C, and the column temperature: 30.0 ℃, the inhibition current generated by the anion auto-electrolysis continuous regeneration micro-membrane suppressor is 90mA, and the operation time is 30min; Resistivity>18.0MΩ·cm, without target ions, filtered through a 0.2μm filter membrane

[0083] (2) Make glyphosate standard curve:

[0084] 1) Store the glyphosate standard stock solution [ρ=100.0mg / L] in a refrigerator at 4°C.

[0085] 2) Glyphosate standard use solution: Take 1.0mL glyphosate standard stock solution, and dilute to 10.0mL with pure water. The standard use solution contains 10.0mg / L glyphosate, and it is newly prepared on the same day.

[...

Embodiment 1-2

[0094] The analysis and detection method of glyphosate in the determination sample of embodiment 1-2

[0095] The operation steps of embodiment 1-2 are the same as that of embodiment 1-1, the difference is that the mobile phase flow rate is 0.8mL / min, the eluent is 20mmol / L sodium hydroxide solution, the temperature of the conductivity cell is 25°C, and the column temperature The temperature is 25°C, the injection volume is 80 μL, the inhibitory current is 80 mA and the analysis time is 20 min.

Embodiment 1-3

[0096] The analytical detection method of glyphosate in the determination sample of embodiment 1-3

[0097] The operation steps of embodiment 1-3 are the same as that of embodiment 1-1, the difference is that the mobile phase flow rate is 0.9mL / min, the eluent is 40mmol / L sodium hydroxide solution, the temperature of the conductivity cell is 35°C, and the column temperature The temperature is 35°C, the injection volume is 120 μL, the inhibitory current is 100 mA and the analysis time is 40 min.

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Abstract

The invention relates to an analysis and detection method for glyphosate in domestic drinking water, and provides an analysis and detection method for glyphosate in drinking water. The analysi and detection method is characterized in comprising the following steps that: (1) determining the operation parameters of an ion chromatograph, wherein the flow velocity of a mobile phase is 0.8-1.0mL / min, and an adopted chromatographic column contains an AS19 analysis column and an AG19 protection column; (2) manufacturing a glyphosate standard curve; and (3) determining the content of the glyphosate ina sample. By use of the method disclosed by the invention, sample pretreatment is not required, instead, the sample directly enters an instrument for analysis, post-column derivatization is not required, so that the method is convenient in operation and easy in implementation, the AS19 analysis column and the AG19 protection column are adopted to enlarge a sample adding amount, a column temperature and the a conductance cell temperature are optimized, and therefore, the method exhibits better practicality and generalization performance. In addition, the analysis and detection method disclosedby the invention has a small standard deviation, adding standard recovery is 98.8-101% and is favorable for detecting a large batch of samples.

Description

technical field [0001] The invention relates to an analysis and detection method for pesticide indicators in drinking water, in particular to an analysis and detection method for glyphosate in drinking water. Background technique [0002] Glyphosate, the potent active chemical ingredient in many widely used herbicides, is heavily regulated in the European Union. Glyphosate is not directly related to GMO crops, and the herbicide glyphosate is also required for non-GMO crops. The European Food Safety Authority (EFSA) and EU member states have completed the reassessment of the herbicide glyphosate. They issued a report stating that glyphosate is likely to have a carcinogenic risk to humans, and also proposed some new measures to strengthen the control of food. Safety measures for glyphosate residues. On October 27, 2017, the list of carcinogens released by the International Agency for Research on Cancer of the World Health Organization was initially compiled for reference, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 赵凯兰晶晶吴玉梅郭伟
Owner 北京市水文总站
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