Method for determining parathion in grain based on dispersive liquid-liquid microextraction of hydrophilic and hydrophobic deep-eutectic solvent in combination with digital image colorimetric method

A low eutectic solvent, liquid dispersion technology, applied in material analysis by observing the effect of chemical indicators, preparation of test samples, analysis by chemical reaction of materials, etc., can meet the professional requirements of technicians High, long detection time, expensive equipment and other problems, to avoid organic solvents, less sample required, and low cost

Active Publication Date: 2022-04-15
SHANXI AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above detection methods can meet the requirements of detection accuracy in terms of specificity and sensitivity, the instruments are complex, expensive, time-consuming, and have high professional requirements for technicians.

Method used

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  • Method for determining parathion in grain based on dispersive liquid-liquid microextraction of hydrophilic and hydrophobic deep-eutectic solvent in combination with digital image colorimetric method
  • Method for determining parathion in grain based on dispersive liquid-liquid microextraction of hydrophilic and hydrophobic deep-eutectic solvent in combination with digital image colorimetric method
  • Method for determining parathion in grain based on dispersive liquid-liquid microextraction of hydrophilic and hydrophobic deep-eutectic solvent in combination with digital image colorimetric method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: verification of experimental feasibility

[0048] Preparation method: Prepare four 1.5 mL centrifuge tubes and configure four different reaction systems: a: parathion + hydrophilic DES; b: parathion + hydrophilic DES + hydrophobic DES; c: parathion + hydrophilic DES+alkali; d: parathion+hydrophilic DES+alkali+hydrophobic DES; measure their UV absorption spectra respectively.

[0049] The experimental results are shown in Figure 3: when the hydrophobic DES and sodium hydroxide do not exist, the a system is colorless. When the hydrophobic DES exists and the sodium hydroxide does not exist, the b system has no obvious change, and the solution is still colorless. When sodium hydroxide exists and hydrophobic DES does not exist, the c system has a weak absorption peak around 410 nm, but the solution is still colorless. When the hydrophobic DES and sodium hydroxide were present at the same time, a significant absorption peak appeared in the d system at around 4...

Embodiment 2

[0050] Example 2: condition optimization

[0051] A. Types of hydrophilic DES

[0052] (1) Experimental method: Accurately weigh 0.1 g of sample into a 0.5 mL centrifuge tube, add 200 μL of hydrophilic DES (choline chloride is synthesized with ethylene glycol, propylene glycol, and butanediol, respectively), and then vortex for 60 s , put it in a centrifuge and centrifuge at 6000r / min for 1min, take out the supernatant and place it in a 0.5 mL centrifuge tube, add 100 μL sodium hydroxide aqueous solution, and then add 100 μL hydrophobic DES, hydrophobic DES can dissociate in situ, dissociated hydrophilic TBA ＋ Under alkaline conditions, the parathion in the hydrophilic DES was converted into a yellow product, which was extracted by the hydrophobic extractant terpineol generated in situ and dispersed in the solution, and centrifuged at 6000r / min for 1min. Remove the lower aqueous phase with a syringe. Then take pictures of the colored part in the centrifuge tube, analyze the...

Embodiment 3

[0081] Embodiment 3: the making of parathion standard curve

[0082] (1) Experimental method: Accurately weigh 0.1 g of sample (addition concentration is 0.01 mg kg -1 , 0.05 mg kg -1 , 0.10 mg kg -1 , 0.50 mg kg -1 , 1.00 mg kg -1 , 2.00 mg kg -1 , 5.00 mg kg -1), add 200 μL of hydrophilic DES (choline chloride and propylene glycol are synthesized by 1 / 3), then vortex extract for 60 s, put it in a centrifuge and centrifuge at 3260 g for 1 min, take out the supernatant and place it in a 0.5 mL centrifuge Add 100 μL sodium hydroxide aqueous solution to the tube, then add 100 μL hydrophobic DES (tetrabutylammonium bromide and terpineol are synthesized by 1 / 1), centrifuge at 3260 g for 1 min, dissolve parathion in pine oil The alcoholic organic phase is located in the upper layer of the centrifuge tube, and the lower aqueous phase is removed with a syringe. Then take pictures of the colored part in the centrifuge tube, and analyze and calculate the RGB value (I). Draw the...

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Abstract

The invention aims to provide a method for determining parathion in grain by combining dispersive liquid-liquid microextraction with digital image colorimetry, belongs to the technical field of food safety detection, and adopts hydrophilic DES as an extraction agent to replace traditional toxic organic solvents such as methanol and acetonitrile to complete extraction of parathion pesticide in grain samples. Hydrophobic DES synthesized by a hydrogen bond acceptor and a hydrogen bond donor according to a certain proportion can be dissociated into TBA < + > and alcohol in situ, parathion in a hydrophilic DES phase is converted into a yellow product by the dissociated hydrophilic TBA < + > under an alkaline condition, and the yellow product is further extracted and purified by a hydrophobic extraction agent alcohol which is generated in situ and dispersed in a solution. And then performing quantitative detection on yellow products in the organic phase by using a digital image colorimetric method. The whole process is simple to operate, low in cost, rapid and sensitive, and has the advantages of avoiding use of organic solvents, saving the dosage of extracting agents, being green and environment-friendly and the like.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and in particular relates to a method for determining parathion in grains based on hydrophilic and hydrophobic deep eutectic solvent dispersion liquid-liquid microextraction combined with digital image colorimetry. Background technique [0002] Parathion is a highly efficient organophosphorus insecticide and acaricide, which is mainly used to control pests and diseases and increase the total yield of crops. However, due to improper use, it will form residues in food, which will have a negative impact on the human body. Parathion pesticide is highly toxic, and its toxicity is based on irreversible inhibition of the activity of acetylcholinesterase in the human body, which is crucial to the central nervous system of the human body. Ingestion through food or long-term exposure can cause symptoms such as headache, vomiting, blurred vision, trance, respiratory paralysis and even death. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N21/78
CPCG01N1/34G01N21/78
Inventor 陈振家张卓婷王晓闻牛宇荆旭
Owner SHANXI AGRI UNIV
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