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Method for on-line determination of sulfonylurea herbicides in water

A technology for sulfonylureas and herbicides, applied in the field of detection of sulfonylureas herbicides, can solve the problems of large limitations, complicated pretreatment, and inability to eliminate false positives, and achieve simple operation, short analysis time, and organic reagents The effect of using less

Pending Publication Date: 2022-01-21
太湖流域水文水资源监测中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2019, the Ministry of Ecology and Environment issued a high-performance liquid chromatography method for the determination of sulfonylurea pesticides in water quality. However, the pretreatment of this method is complex and has great limitations. The analysis time of a single sample is about 100 minutes, and problems such as false positives cannot be eliminated.

Method used

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  • Method for on-line determination of sulfonylurea herbicides in water
  • Method for on-line determination of sulfonylurea herbicides in water
  • Method for on-line determination of sulfonylurea herbicides in water

Examples

Experimental program
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Embodiment 1

[0049] A method for online determination of sulfonylurea herbicides in water, comprising:

[0050] Sample collection, configuration of an online solid phase extraction system and configuration of a triple quadrupole compound linear ion trap mass spectrometer; the configuration of the triple quadrupole compound linear ion trap mass spectrometer includes: adding information-dependent acquisition and enhanced Product ion scan, and scan the standard substance, use the obtained enhanced product ion full-scan mass spectrum to establish a standard substance spectral library.

[0051] Configure the standard curve for the standard solution according to the configured online solid-phase extraction system; filter, enrich and purify the sample to obtain a purified product, and elute and separate the purified product;

[0052] The purified substances are detected according to the configured triple quadrupole compound linear ion trap mass spectrometer.

[0053] Specifically, the instrument...

Embodiment 2

[0071] Such as figure 1 As shown, the configuration of the online solid-phase extraction system is specifically:

[0072] The online solid-phase extraction system includes 2 high-pressure quaternary pumps, 1 thermostatic column oven, 1 54-bit 4mL sample tray, 1 54-bit filter membrane tray, 1 99-bit 2mL sample tray, and 1 32-bit 10mL sample tray. Sample tray, 1 automatic needle changing device, the first injection arm connected with the filter needle, the second injection arm connected with the injection needle, a 3-position 100mL needle washing solution sample tray, 4 six-way valves, HLB on-line solid phase extraction column SPE1, HLB on-line solid phase extraction column SPE2, a chromatographic column whose packing is C18, the HLB on-line solid phase extraction column SPE1 and the HLB on-line solid phase extraction column SPE2 can be used in parallel, in which When one is eluted for analysis, the other starts to activate and enrich the sample; the six-way valve includes valv...

Embodiment 3

[0093] According to the configuration of the online solid phase extraction system, the standard curve is configured for the standard solution, and the sample is filtered, enriched and purified on-line to obtain a purified substance, and the purified substance is eluted and separated. Specifically, the sample is Add it into a 10mL sample bottle, filter through the online filter device in the configured online solid phase extraction system, and enrich, purify, elute, and separate the filtered sample through an online solid phase extraction column.

[0094] Wherein, the elution and separation include:

[0095] Separation by Kinetex C18 column;

[0096] Gradient elution is carried out by a mixture of mobile phase acetonitrile and mobile phase 0.1% formic acid aqueous solution;

[0097] The configuration of the elution conditions is specifically: the mobile phase is 0.1% formic acid water and the mobile phase acetonitrile are mixed in proportion, and the flow rate is 0.4mL / min; th...

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Abstract

The invention relates to the technical field of sulfonylurea herbicide detection, in particular to a method for on-line determination of sulfonylurea herbicides in water, which comprises the steps of sample collection, configuration of an on-line solid phase extraction system and configuration of a triple quadrupole composite linear ion trap mass spectrometer, and further comprises the following steps: adding information dependence acquisition and enhanced daughter ion scanning on the basis of multi-reaction monitoring, scanning a standard substance, and establishing a standard substance spectrum library by using an obtained enhanced daughter ion full-scanning mass spectrum; performing standard curve configuration on the standard solution; and carrying out on-line filtration and enrichment purification on the sample to obtain a purified substance, eluting and separating the purified substance, and finally detecting. The method has the advantages of simple operation, direct on-line sample analysis, short analysis time, less organic reagent dosage and high method sensitivity. In addition, the online solid-phase extraction and linear ion trap technology effectively reduces experimental errors caused by factors such as human interference and matrix interference, and the precision and accuracy of the method can be effectively improved.

Description

technical field [0001] The invention relates to the technical field of detection of sulfonylurea herbicides, in particular to a method for online determination of sulfonylurea herbicides in water. Background technique [0002] Sulfonylurea herbicides are herbicides with high activity, broad spectrum, strong selectivity and low mammalian toxicity. They have been widely used in wheat, rice, corn, soybean, rapeseed, sugar beet, sugarcane, lawn, etc. crop weeding, accounted for 3.7% of the global pesticide market as of 2014. In recent years, studies have found that sulfonylurea herbicides are difficult to degrade in the environment and have certain health risks. The Ministry of Agriculture of my country began to restrict the production and use of metsulfuron-methyl, chlorsulfuron-methyl and anisulfuron-methyl in 2013. [0003] Taihu Lake is the third largest freshwater lake in my country, and it is also an important source of drinking water in the Taihu Lake Basin. There are n...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72
Inventor 徐枫虞霖吴圣明陈方徐佳杭代倩子沈一波
Owner 太湖流域水文水资源监测中心
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