Method for detecting residual quantity of orthocide in vegetables and fruits

A detection method, the technology of captandan, is applied in the detection of captanidan residues in vegetables and fruits, and the detection of pesticide residues. The effect of improving sensitivity, improving recovery, and easy operation

Active Publication Date: 2015-07-29
INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both literature (2007.3, vol.25 No2, 226-229) and literature (2007.9, vol., 13 No9) used phosphoric acid solution for sample treatment, adding acetic acid-sodium acetate buffer solution to the mobile phase for detection by HPLC UV detector , the method has low sensitivity and high detection limit, and has certain requirements on th

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  • Method for detecting residual quantity of orthocide in vegetables and fruits
  • Method for detecting residual quantity of orthocide in vegetables and fruits
  • Method for detecting residual quantity of orthocide in vegetables and fruits

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Example 1: Detection of captan residues in apples

[0044] (1) Sample pretreatment

[0045] Weigh 10.0 g of well-mixed apples into an Erlenmeyer flask, add 8 mL of acetic acid-sodium acetate buffer (pH=4) solution and mix well, add 100 mL of acetone to homogenize and extract for 3 minutes, filter with suction, and transfer the filtrate to a flat bottom flask In the filter residue, add 50 mL of acetone to homogenize extraction for 3 min, filter with suction, and combine the filtrate. Concentrate to about 30mL. Transfer the concentrated solution to a separatory funnel containing 50 mL of 10% sodium chloride solution, rinse the flat-bottomed flask with 50 mL of petroleum ether and transfer to the separatory funnel, shake vigorously for 2 minutes, stand for separation, and take the upper organic layer over anhydrous sodium sulfate Phase in the flat-bottomed flask, the lower aqueous phase was extracted again with 30 mL petroleum ether, the organic phases were combined, concentr...

Embodiment 2

[0068] Example 2 Detection of captan residue in cucumber

[0069] (1) Sample pretreatment

[0070] Weigh 15.0 g of well-mixed cucumber into an Erlenmeyer flask, add 8 mL of acetic acid-sodium acetate buffer (pH=2.6) solution and mix well, add 60 mL of acetone to homogenize and extract for 3 minutes, filter with suction, and transfer the filtrate to a flat bottom flask In the filter residue, add 30 mL of acetone to homogenize extraction for 3 min, filter with suction, and combine the filtrate. Concentrate to about 30mL. Transfer the concentrated solution to a separatory funnel containing 50 mL of 10% sodium chloride solution, rinse the flat-bottomed flask with 50 mL of petroleum ether and transfer to the separatory funnel, shake vigorously for 2 minutes, stand for separation, and take the upper organic layer over anhydrous sodium sulfate Phase in the flat-bottomed flask, the lower aqueous phase was extracted again with 30 mL petroleum ether, the organic phases were combined, conce...

Embodiment 3

[0083] Add 8 mL of acetic acid-sodium acetate buffer solution (pH=4.8) and mix well, add 100 mL of acetone for homogenization and extract for 3 min, filter with suction, transfer the filtrate to a flat-bottomed flask, and add 50 mL of acetone to the filter residue for homogenization and extract for 3 min. Filter with suction and combine the filtrate. Concentrate to about 30mL. Transfer the concentrated solution to a separatory funnel containing 50 mL of 10% sodium chloride solution, rinse the flat-bottomed flask with 50 mL of petroleum ether and transfer to the separatory funnel, shake vigorously for 2 minutes, stand for separation, and take the upper organic layer over anhydrous sodium sulfate Phase in the flat-bottomed flask, the lower aqueous phase was extracted again with 30 mL petroleum ether, the organic phases were combined, concentrated to about 3 mL, and then passed through the column. The Florisil cartridge is pre-leached with 5 mL of n-hexane, the concentrated solut...

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Abstract

The invention discloses a method for detecting the residual quantity of orthocide in vegetables and fruits. The method is realized through the following steps of homogeneously extracting residual orthocide in a sample by using an acetic acid-sodium acetate buffer solution (pH 2.6 to 4.8) and acetone, after a concentrated solution is purified through liquid-liquid extraction and a Florisil solid-phase extraction column (Florisil), detecting the purified concentrated solution through a gas chromatography-electron capture detector (GC-ECD), and quantifying through an external standard method. By using the method, the average recovery rate is 90.1% to 108.6%; the average relative standard deviation (RSD) is 1.5% to 5.5%; the lowest detection limit is 0.005mg/kg; the method has the advantages of good repeatability, high sensitivity, simpleness and convenience in operation and accurate and quick quantification. The technical requirements that maximum residue limits of the orthocide in the fruits and the vegetables are 0.02mg/kg and 0.05mg/kg in European Union and American can be met, and the powerful technical support is provided for guaranteeing the food security of Chinese people and the sound development of export trade abroad.

Description

Technical field [0001] The invention relates to a method for detecting pesticide residues, in particular to a method for detecting captan residues in vegetables and fruits, and belongs to the technical field of pesticide residue determination. Background technique [0002] Captan, chemical name: N-trichloromethylsulfanyl-1,2,3,6-tetrahydrophthalimide, molecular formula C 9 H 8 Cl 3 NO 2 S, chemical structural formula: [0003] [0004] Captan is a broad-spectrum protective fungicide of trichloromethylthio (SCC 13) developed by Tomian, Japan. It has good control effect and low phytotoxicity. It can stimulate plant growth when used appropriately. Its main mechanism is to block the respiratory process of pathogenic fungi. Captan can be mixed with many conventional pesticides, so it is widely used in crops such as vegetables and fruits. [0005] Although captan has low toxicity to mammals, ruminants, especially sheep, are particularly sensitive to it, with a lethal LD50 of 250 mg / kg. ...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 李瑞娟于建垒宋国春刘同金李如美赵亚
Owner INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI
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