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Preparation method of sodium fluoroacetate for qualitative and quantitative analysis of forensic science

A technology of sodium fluoroacetate and crude sodium fluoroacetate, applied in the field of forensic toxicological analysis, can solve the problems of inability to purchase from the market, homicide and suicide cases still exist, and the toxicity of sodium fluoroacetate is high, achieving high yield and easy operation. , the effect of improving purity and yield

Inactive Publication Date: 2017-07-14
INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to the great toxicity of sodium fluoroacetate, its sale was banned by the relevant departments in 2003; however, due to its obvious effect of killing rodents in agricultural production, it is still sold in the market, especially on the stalls in the rural market, resulting in homicide and Suicides still exist
In order to accurately identify whether the poison exists in the body, it is necessary to use standard or reference substances for qualitative and quantitative detection; however, the standard substances of the above two substances cannot be purchased from the market. For inspection and identification, it is urgent to synthesize and prepare sodium fluoroacetate and fluoroacetic acid in the field of forensic toxicology analysis in the laboratory

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for preparing sodium fluoroacetate for qualitative and quantitative use in forensic science, comprising the steps of: (1) preparing crude sodium fluoroacetate;

[0031] (1-1) Dissolve 141 mmol, 13.6 mL of ethyl fluoroacetate or methyl fluoroacetate in 240 mL of ethanol;

[0032] (1-2) Add 155mmol and 6.2g of NaOH, and stir at 50°C for 12 hours to form a white precipitate;

[0033] (1-3) Remove the solvent under reduced pressure to dryness to obtain crude sodium fluoroacetate solid, wash the obtained crude sodium fluoroacetate solid with 30 mL of methyl tert-butyl ether three times, remove organic impurities and unreacted raw materials, and dry;

[0034] (II) preparing fluoroacetic acid;

[0035] (2-1) adding crude sodium fluoroacetate to hydrochloric acid with an HCl concentration of 3 mol / L, adjusting the pH value of the solution to 4, and adding NaCl to saturation;

[0036] (2-2) were extracted 4 times with 100mL methyl tert-butyl ether, and the organic lay...

Embodiment 2

[0040] The preparation method of sodium fluoroacetate for qualitative and quantitative use in forensic science comprises the following steps:

[0041] (1) preparing crude sodium fluoroacetate;

[0042] (1-1) Dissolve 13.6mL (141mmol) of ethyl fluoroacetate or methyl fluoroacetate in 200mL of methanol;

[0043] (1-2) Add 6.72g (168mmol) of NaOH, stir at room temperature for 20 hours, and slowly form a white precipitate;

[0044] (1-3) Then the solvent was removed under reduced pressure to dryness to obtain crude sodium fluoroacetate, and the obtained crude sodium fluoroacetate solid was washed three times with 30 mL of methyl tert-butyl ether to remove organic impurities and unreacted raw materials, and dried.

[0045] (II) preparing fluoroacetic acid;

[0046] (2-1) Dissolving the crude sodium fluoroacetate in hydrochloric acid with an HCl concentration of 3mol / L, and adding NaCl to saturation;

[0047] (2-2) Then extract 4 times with 100mL methyl tert-butyl ether respectiv...

Embodiment 3

[0051] The preparation method of sodium fluoroacetate for qualitative and quantitative use in forensic science comprises the following steps:

[0052] (1) preparing crude sodium fluoroacetate;

[0053](1-1) Dissolve 13.6 mL (141 mmol) of ethyl fluoroacetate or methyl fluoroacetate in 200 mL of a mixed solution of isopropanol and n-butanol, the volume ratio of isopropanol and n-butanol is 1:1;

[0054] (1-2) Add 6.72g (168mmol) of NaOH, stir at room temperature for 20 hours, and slowly form a white precipitate;

[0055] (1-3) Then the solvent was removed under reduced pressure to dryness to obtain crude sodium fluoroacetate, and the obtained crude sodium fluoroacetate solid was washed three times with 30 mL of methyl tert-butyl ether to remove organic impurities and unreacted raw materials, and dried.

[0056] (II) preparing fluoroacetic acid;

[0057] (2-1) Dissolving the crude sodium fluoroacetate in hydrochloric acid with an HCl concentration of 3mol / L, and adding NaCl to ...

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Abstract

The invention discloses a preparation method of sodium fluoroacetate for qualitative and quantitative analysis of forensic science. The method comprises the following steps: (I) preparing coarse sodium fluoroacetate; (II) preparing fluoroacetic acid; and (III) preparing pure sodium fluoroacetate: dissolving the obtained fluoroacetic acid in a mixed solution of ethanol and water in a volume ratio of 10: 1, then dropwise adding a saturated sodium hydroxide solution into the mixed solution, wherein the amount of substance of sodium hydroxide in the saturated sodium hydroxide solution is 1.05-1.10 times of that of the fluoroacetic acid substance in the mixed solution, and stirring, filtering and drying the mixed solution to obtained pure sodium fluoroacetate. The preparation method of sodium fluoroacetate for qualitative and quantitative analysis of forensic science disclosed by the invention is high in yield, and the prepared fluoroacetic acid is high in purity, and can be directly used as a standard product or a reference product, so that the demand on toxicological analysis of forensic science is met in reality.

Description

technical field [0001] The invention relates to the field of forensic toxicology analysis. More specifically, it relates to a method for preparing fluoroacetic acid used in the field of forensic toxicology analysis. Background technique [0002] Due to the great toxicity of sodium fluoroacetate, its sale was banned by the relevant departments in 2003; however, due to its obvious effect of killing rodents in agricultural production, it is still sold in the market, especially on the stalls in the rural market, resulting in homicide and Suicides persist. In order to accurately identify whether the poison exists in the body, it is necessary to use standard or reference substances for qualitative and quantitative detection; however, the standard substances of the above two substances cannot be purchased from the market. For inspection and identification, it is urgent to synthesize and prepare sodium fluoroacetate and fluoroacetic acid used in the field of forensic toxicology an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/02C07C53/18C07C51/48C07C51/47C07C51/41C07C27/02
CPCC07C51/02C07C51/09C07C51/42C07C51/47C07C51/48C07C53/18
Inventor 杜鸿雁于忠山宋歌徐小英董颖魏春明王瑞花张蕾萍任昕昕
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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