Method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing

A technology of bright photobacteria and high-performance thin-layer chromatography, which is applied in the determination/inspection of microorganisms, chemiluminescence/bioluminescence, biochemical equipment and methods, etc., can solve captan decomposition, difficult captan accurate analysis, false Negative results etc.

Inactive Publication Date: 2019-06-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the addition of this reagent may cause the pH of the extraction solution to rise to neutral or slightly alkaline conditions (pH=7-9), which eventually leads to the decomposition of captan and false negative results
It can be seen that the existence of the above problems makes it difficult for the traditional column chromatography method to accurately analyze captan.

Method used

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  • Method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing
  • Method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing
  • Method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of captan standard solution: use ethyl acetate as a solvent to prepare a standard solution of captan with a concentration of 0.01 mg / mL, and then to establish a standard curve, the standard solution needs to be diluted to 0.001 and 0.0005 mg / mL ;

[0026] (2) High-efficiency thin-layer chromatography separation: 4-8μL captan standard, apple, pear and cherry samples were accurately spotted with Linomat 5, and after spotting was completed, a developing solution (toluene: ethyl acetate = 8: 2 (v / v)) unfolding, the upward unfolding distance is 60 mm, after the unfolding is completed, take out the silica gel plate and place it on a flat heater at 100°C for 5 minutes to fully dry;

[0027] (3) Imaging with a bioluminescence imager: the high-performance thin-layer chromatography plate in step (2) is dipped to couple the suspension of Bright Bacteria with the chromatographic separation results, and then placed in a bioluminescence imager for imaging;

[0028] (...

Embodiment 2

[0031] The specific implementation method is the same as in Example 1, the difference is that the selection of the mobile phase for development, the test toluene:ethyl acetate=8:2 (v / v) has the best development effect, and then the matrix effect experiment is carried out with the same ratio of mobile phase. There is no obvious difference in the development effect, indicating that the sample matrix has no obvious interference on the development, and this mobile phase is used for the development of the recovery of the standard addition.

Embodiment 3

[0033] (1) Apples, pears and cherries and different spiked quantities were tested separately.

[0034] For the pretreatment of fruits: apples, pears and cherries: add 10 g of fruit sample homogenate to a 50 mL centrifuge tube, continue to add 10 mL of acetonitrile, 0.1 mL of formic acid, shake and mix, ultrasonic water bath for 10 min; then add 4 g Anhydrous magnesium sulfate and 1 g of anhydrous sodium acetate, shake and mix well, centrifuge at 4000r / min for 5 min, take 2-4 mL of the upper acetonitrile phase, and pass through a 0.45 μm filter membrane to obtain a liquid sample that can be directly used for analysis. Refrigerate it at 4°C.

[0035] Pretreatment of the sample solution of the recovery rate of the standard addition: add 10 g of the homogenate of the fruit sample into a 50 mL centrifuge tube, continue to add 10 mL of acetonitrile, 0.1 mL of formic acid, oscillate and mix, and ultrasonically bathe for 10 min; then add 4 g of anhydrous magnesium sulfate and 1 g of ...

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Abstract

The invention discloses a method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing,and belongs to the technical field of the food detection. The method comprises the following steps: firstly performing sample preparation and sample cleaning on fruit homogenate through solid-liquidextraction, and then developing an extract through high-performance thin-layer chromatography, enabling the target captan to separate from a sample interference matrix substance in extraction liquid,and then coupling a chromatographic separation result with the photobacterium phosphoreum biosensing through a dipping manner; and quantitatively assessing the target captan residue concentration in the fruit by combining the bioluminescence autography with digital image analysis. The invention establishes a method for quickly and quantitatively screening captan residue in fruit through high-performance thin-layer chromatography coupled with photobacterium phosphoreum biosensing, the method has the advantages of being quick, accurate and economic; and meanwhile, the method example for quicklyand reliably screening harmful substance residue with invisible spectrum characteristic in the food is provided based on the establishment of the high-performance thin-layer chromatography and bioluminescence autography coupled detection method.

Description

technical field [0001] The invention relates to a method for rapid and quantitative screening of captan residues in fruits by high-efficiency thin-layer chromatography combined with biosensing of luminescent bacteria, and belongs to the technical field of food detection. Background technique [0002] Captan (N-(trichloromethylthio)-4-cyclohexene-1,2-dicarboximide), which belongs to organosulfur substances, is one of the broad-spectrum fungicides most widely used for plant protection purposes in agricultural production. Especially for various fruits and vegetables after harvest, captan has good freshness preservation performance, which can ensure that the fruits still have a fresh and healthy appearance after storage and processing. Nonetheless, the potential public health risks associated with the misuse of captan have been noted. Recent studies have demonstrated that, in addition to symptoms of acute toxicity such as vomiting and conjunctivitis, exposure to captan even at ...

Claims

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Application Information

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IPC IPC(8): G01N30/90G01N21/76C12Q1/02
Inventor 陈益胜舒蓝萍王了徐学明张煌黄彩虹金征宇谢正军柏玉香
Owner JIANGNAN UNIV
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