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Pre-treating and detecting method for sample containing dithiocarbamate compound

A technology of dithiocarbamic acid and ester compounds, which is applied in the field of detection and analysis, and can solve problems such as high requirements for operators, risks to the environment and the health of operators, and many influencing factors

Active Publication Date: 2016-11-16
CHINA TOBACCO FUJIAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] First, the reaction conditions of ultrasonic heating are relatively severe, and part of the carbon disulfide produced by the reaction evaporates in gaseous form and cannot be extracted by isooctane, resulting in low detection results;
[0005] Second, carbon disulfide distributes and dissolves in a certain proportion in the two phases of water and isooctane, but does not completely dissolve in isooctane, resulting in low detection results. At the same time, the distribution of the dissolution ratio is affected by factors such as temperature, which makes the detection results poor stability;
[0006] Third, the operation steps are cumbersome, there are many influencing factors, and the requirements for operators are relatively high;
[0007] Fourth, the volatilization of isooctane under high temperature conditions poses risks to the environment and the health of operators

Method used

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  • Pre-treating and detecting method for sample containing dithiocarbamate compound
  • Pre-treating and detecting method for sample containing dithiocarbamate compound
  • Pre-treating and detecting method for sample containing dithiocarbamate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] refer to figure 1 For the process, set the ambient temperature to 38.5°C to ensure that the entire pretreatment and detection process is carried out at this temperature.

[0072] 1. Sample pretreatment

[0073] Dry the tea sample at 40°C for 24 hours, weigh 0.5g of the tea sample and put it into a 100mL conical flask, add 20mL of an ethanol solution containing 0.5mol / L tin protochloride with a pH value of 6, and spin at 60 rpm The rate of magnetic stirring was 0.5 hours, and after standing for 10 minutes, the solid-liquid separation was performed to obtain a solution.

[0074] 2. Detection

[0075] Take 1mL of the solution, and carry out a color reaction with 1mL of an ethanol solution containing 0.05mol / L copper acetate and 0.01mol / L diethylamine to obtain a sample solution containing the chromogenic substance copper diethylaminodithioformate.

[0076] Use a spectrophotometer to measure the absorbance of the sample solution at 272nm, 302nm and 332nm, and obtain the ...

Embodiment 2

[0083] refer to figure 1 For the process, set the ambient temperature to 40°C to ensure that the entire pretreatment and detection process is carried out at this temperature.

[0084] 1. Sample pretreatment

[0085] Dry the tobacco powder sample at 40°C for 24 hours, weigh 0.75g of the tobacco powder sample and pack it into a 100mL conical flask, add 22.5mL of ethanol solution containing 0.75mol / L tin protochloride with a pH value of 5.5, and Stir magnetically at a rate of 75 rpm for 0.75 hours, and after standing still for 15 minutes, separate the solid and liquid to obtain a solution.

[0086] 2. Detection

[0087] Take 1.5 mL of the solution, and carry out a color reaction with 1.5 mL of ethanol solution containing 0.75 mol / L copper acetate and 0.25 mol / L diethylamine to obtain a sample solution containing the chromogenic substance copper diethylaminodithiocarbamate.

[0088] Referring to the method in Example 1, the content of the chromogenic substance in the sample sol...

Embodiment 3

[0092] refer to figure 1 Process, the ambient temperature is 41.5°C, and the entire pretreatment and detection process is guaranteed to be carried out at this temperature.

[0093] 1. Sample pretreatment

[0094] Dry the apple sample at 40°C for 24 hours, weigh 1g of the apple sample and put it into a 100mL conical flask, add 25mL of an ethanol solution containing 1mol / L stannous chloride with a pH value of 5, and rotate at 90 rpm Speed ​​magnetic stirring for 1 hour, after standing still for 20 minutes, solid-liquid separation to obtain a solution.

[0095] 2. Detection

[0096] Take 2mL of the solution, and carry out a color reaction with 2mL of ethanol solution containing 0.1mol / L copper acetate and 0.04mol / L diethylamine to obtain a sample solution containing the chromogenic substance copper diethylaminodithioformate.

[0097] With reference to the method in Example 1, detect the chromogenic substance content in the sample solution by spectrophotometry, obtain the conte...

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Abstract

The invention belongs to the field of detection analysis and relates to a pre-treating method for a sample containing a dithiocarbamate compound. The method comprises the following steps: mixing a sample with an acidic stannous chloride ethanol solution and separating, thereby acquiring a solution containing carbon disulfide; optionally, standing by after the mixing and before separating. The invention further relates to a method for detecting the dithiocarbamate compound in the sample. According to the method provided by the invention, the content of dithiocarbamate compound in the sample can be accurately determined, the stability is high, the operation is simple and convenient and the method is clean and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of detection and analysis, and in particular relates to a pretreatment method for samples containing dithiocarbamate compounds, and also relates to a method, kit and application for detecting dithiocarbamate compounds in samples. Background technique [0002] Dithiocarbamate compounds are a general term for a class of organosulfur pesticides, which are divided into thirams and dysons. Because of their broad-spectrum and high-efficiency bactericidal effects, they are widely used in tobacco, food, vegetables, fruit trees, cotton, etc. in disease control. However, with the wide application of dithiocarbamate compounds, it is found that a metabolite called ethylenethiourea (ETU) is produced in the metabolic process of crops, food, animals and plants that have been applied with it, and its chemical name is For tetrahydroimidazole-2-thione. According to reports, ETU has carcinogenicity, teratogenicity and mutagenicity, ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N21/31G01N21/78
CPCG01N1/28G01N21/31G01N21/78
Inventor 吴清辉谢卫刘泽春黄朝章张建平许寒春刘江生黄延俊邓其馨黄华发李巧灵
Owner CHINA TOBACCO FUJIAN IND
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