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Method for detecting regulating-agent thidiazuron residues and regulating-agent diuron residues

A technology for thidiazuron and diuron is applied in the field of detecting the residues of regulators thidiazuron and diuron, which can solve problems such as residues, and achieve the effects of satisfying the detection limit, simple purification, and satisfactory precision.

Inactive Publication Date: 2015-12-30
河南省农业科学院农业质量标准与检测技术研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the chronic toxicity test, the ineffective dose for rats is 250 mg / kg (2 years), and the ineffective dose for dogs is 125 mg / kg (1 year). Both are used as pesticides, and after use, there are often residues

Method used

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  • Method for detecting regulating-agent thidiazuron residues and regulating-agent diuron residues
  • Method for detecting regulating-agent thidiazuron residues and regulating-agent diuron residues
  • Method for detecting regulating-agent thidiazuron residues and regulating-agent diuron residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Weigh 20.0g of the prepared cotton leaf sample (accurate to 0.01g) into a 200mL glass bottle, add 10mL of water and 50mL of acetonitrile, mix thoroughly, ultrasonically extract for 20min, and filter with filter paper until 3g of sodium chloride is added. In a stoppered measuring cylinder, shake vigorously for 1 min, and after standing for 1 h, accurately pipette 25 mL of supernatant into a 100 mL beaker, place on a heating plate, and blow with nitrogen at 50 °C to nearly dry.

Embodiment 2

[0057] Weigh about 5.0 g of soil samples and dry them at 105°C to constant weight to measure the water content in the soil. Then accurately weigh 20.0 g of the prepared soil sample (accurate to 0.01 g) into a 100 mL centrifuge tube, add 10 mL of water and 50 mL of acetonitrile, vortex for 1 min, sonicate for 20 min, and centrifuge at 4000 r / min for 5 min. The supernatant was filtered through filter paper into a stoppered measuring cylinder added with 3g of sodium chloride, shaken vigorously for 1min, and after standing for 1h, accurately pipette 25mL of the supernatant into a 100mL beaker, placed on a heating plate, and blown with nitrogen at 50°C near Dry.

Embodiment 3

[0059] Accurately weigh 10.0g (accurate to 0.01g) of the prepared cottonseed sample into a 100mL centrifuge tube, add 10mL water and 50mL acetonitrile, vortex for 1min, sonicate for 20min, and centrifuge at 4000r / min for 5min. The supernatant was filtered through filter paper into a stoppered measuring cylinder added with 3g of sodium chloride, shaken vigorously for 1min, and after standing for 1h, accurately pipette 25mL of the supernatant into a 100mL beaker, placed on a heating plate, and blown with nitrogen at 50°C near Dry.

[0060] C 18 The column was pre-rinsed with 5mL ethyl acetate, 5mL ethyl acetate dissolved the sample residue, and transferred to the column, then eluted with 10mL ethyl acetate, the eluate was collected, and placed on an electric heating plate at 35°C and blown with nitrogen to dry it. . Accurately dilute to 2mL with methanol, and filter through a 0.22μm needle-hole filter into a 2mL injection vial for testing.

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Abstract

The invention discloses a method for detecting regulating-agent thidiazuron residues and regulating-agent diuron residues. The method is characterized by including the following steps that after a C18 column is pre-rinsed through 5 ml of ethyl acetate, sample residues obtained through filtering carried out after ultrasonic extraction are dissolved through 5 ml of ethyl acetate; the mixture is transferred to the column and eluted through 10 ml of ethyl acetate, and eluent is collected, arranged on an electric heating plate and blown through nitrogen at the temperature of 35 DEG C to be approximately dry; the volume of the obtained product is accurately fixed to 2 mL through methyl alcohol, and the mixture is filtered into a 2-mL small sample injection bottle through a 0.22-micron needle hole filtering film; the obtained sample flows through a chromatographic column at the flowing speed of 1.0 mL / min, and detection is carried out through a liquid chromatograph and a PDA detector. According to the method, 50 mL of acetonitrile serves as extracting liquid; compared with the reported mode that acetone serves as extracting liquid, the use amount is small, and later-period purification is simple; compared with the mode that methyl alcohol serves as extracting liquid, after extracting and salting-out are carried out, the mixture is distilled to be dry through the heating plate, rotary steaming is avoided, and working efficiency can be improved.

Description

technical field [0001] The invention relates to the field of pesticide detection, in particular to a method for detecting residues of modulators thiadizuron and diuron. Background technique [0002] The toxicity of thiadizuron is: Acute oral LD ​​of the original drug in rats 50 : Mouse>5000mg / kg, rat>4000mg / kg. Rabbit Mild eye irritation, no skin irritation. No skin sensitization in guinea pigs; acute inhalation of LC in rats 50 (4h)>2.3mg / L; the toxicity of diuron is: acute oral LD ​​of the original drug in rats 50 It is 3400mg / kg, and it is irritating to eyes and mucous membranes at high concentrations. In the chronic toxicity test, the ineffective dose for rats is 250 mg / kg (2 years), and the ineffective dose for dogs is 125 mg / kg (1 year). Both are used as pesticides, and after use, there will often be residues. Contents of the invention [0003] In order to solve the above problems, the present invention provides a method for detecting residues of modula...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 吴绪金张军锋马婧玮周玲李萌刘进玺李通祁玉峰周娟马欢刘丹黎俎建英董小海
Owner 河南省农业科学院农业质量标准与检测技术研究所
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