Method of extracting medicine residues of sulfonamides from chicken by utilization of ionic liquid

Abstract

The invention relates to a method of extracting medicine residues of seven sulfonamides from chicken by utilization of an ionic liquid and achieving an objective of purification during extraction purification, through adjusting the pH value, the water amount and the salt amount in the ionic liquid to achieve homogeneous phase extraction and layered purification, wherein the seven sulfonamides residues comprise sulfathiazole (ST), sulfamerazine (SMR), sulfamethizole (STZ), sulfadimidine (SDMD), sulfachlorpyridazine (SCP), sulfamethoxazolum (SMZ), and sulfisoxazole (SIX). Liquid chromatographic analysis results show that the recovery rate of each of the sulfonamides is 82.1%-108%, and the relative standard deviation is 0.5%-5.9%. The green and simple extracting method is established so as to reduce pollution or harm of traditional organic solvent extraction methods to the environment and to experiment persons.

Description

technical field

[0001] The invention belongs to the technical field of ionic liquid extraction and separation. Specifically, the invention relates to an ionic liquid that is odorless, non-flammable, non-volatile, and has good solubility characteristics, by adjusting the pH value and adding a certain amount of salt, so as to achieve the purpose of extraction in a homogeneous state, and then layered purification, Therefore, a simple and green extraction method is established to replace the traditional volatile organic solvent extraction method. Background technique

[0002] The commonly used methods for the determination of sulfonamide residues are mainly liquid chromatography and liquid chromatography tandem mass spectrometry. In these methods, sulfonamides are all extracted with organic solvent acetonitrile, the toxicity is relatively large, and the acute toxicity is LD 50 2730mg / kg (rat oral); 1250mg / kg (rabbit dermal); LC 50 12663mg / m 3 If people inhale more than 500pp...

Examples

Embodiment 1

[0041] The method of the present invention is used to extract sulfonamides in Wenchang chicken, and the steps of the method are as follows:

[0042] Commercially available Wenchang chicken was made into a homogenate state with a blender, 2 g was taken and put into a 10 mL polypropylene tube, and a series of standard solutions of different concentrations were added.

[0043] (1) Preparation of extract

[0044] Put water, 1-hexyl-3-methylimidazolium tetrafluoroborate and glacial acetic acid into a container at a ratio of 5:1:0.1, stir evenly, make the water phase and the ionic liquid miscible, and become a homogeneous phase, as Chicken sulfa drug residue extract.

[0045] (2) High-speed dispersion

[0046] Heat 6mL of the extract obtained in step (1) to 30-40°C, add it to about 2 grams of chicken, and then use a high-speed disperser at 4000-8000rpm (preferably 5000-7000rpm) to disperse for 60-90s, and vortex After ultrasonic extraction for 3 minutes, centrifuge for 5 minutes ...

Embodiment 2

[0058] The method of the present invention is used to extract the sulfonamide in the three-yellow chicken, and the steps of the method are as follows:

[0059] Commercially available Wenchang chicken was made into a homogenate state with a blender, 2 g was taken and put into a 10 mL polypropylene tube, and a series of standard solutions of different concentrations were added.

[0060] (1) Preparation of extract

[0061] Put water, 1-hexyl-3-methylimidazolium tetrafluoroborate and glacial acetic acid into a container at a ratio of 5:1:0.1, stir evenly, make the water phase and the ionic liquid miscible, and become a homogeneous phase, as Chicken sulfa drug residue extract.

[0062] (2) High-speed dispersion

[0063] Heat 6mL of the extract obtained in step (1) to a temperature of 30-40°C, add it to about 2 grams of chicken, and then use a high-speed disperser at 4000-8000rpm (preferably 5000-7000rpm) to disperse for 60-90s, and vortex After ultrasonic extraction for 3 minute...

technical field

[0001] The invention belongs to the technical field of ionic liquid extraction and separation. Specifically, the invention relates to an ionic liquid that is odorless, non-flammable, non-volatile, and has good solubility characteristics, by adjusting the pH value and adding a certain amount of salt, so as to achieve the purpose of extraction in a homogeneous state, and then layered purification, Therefore, a simple and green extraction method is established to replace the traditional volatile organic solvent extraction method. Background technique

[0002] The commonly used methods for the determination of sulfonamide residues are mainly liquid chromatography and liquid chromatography tandem mass spectrometry. In these methods, sulfonamides are all extracted with organic solvent acetonitrile, the toxicity is relatively large, and the acute toxicity is LD 50 2730mg / kg (rat oral); 1250mg / kg (rabbit dermal); LC 50 12663mg / m 3 If people inhale more than 500pp...

Examples

Embodiment 1

[0041] The method of the present invention is used to extract sulfonamides in Wenchang chicken, and the steps of the method are as follows:

[0042] Commercially available Wenchang chicken was made into a homogenate state with a blender, 2 g was taken and put into a 10 mL polypropylene tube, and a series of standard solutions of different concentrations were added.

[0043] (1) Preparation of extract

[0044] Put water, 1-hexyl-3-methylimidazolium tetrafluoroborate and glacial acetic acid into a container at a ratio of 5:1:0.1, stir evenly, make the water phase and the ionic liquid miscible, and become a homogeneous phase, as Chicken sulfa drug residue extract.

[0045] (2) High-speed dispersion

[0046] Heat 6mL of the extract obtained in step (1) to 30-40°C, add it to about 2 grams of chicken, and then use a high-speed disperser at 4000-8000rpm (preferably 5000-7000rpm) to disperse for 60-90s, and vortex After ultrasonic extraction for 3 minutes, centrifuge for 5 minutes ...

Embodiment 2

[0058] The method of the present invention is used to extract the sulfonamide in the three-yellow chicken, and the steps of the method are as follows:

[0059] Commercially available Wenchang chicken was made into a homogenate state with a blender, 2 g was taken and put into a 10 mL polypropylene tube, and a series of standard solutions of different concentrations were added.

[0060] (1) Preparation of extract

[0061] Put water, 1-hexyl-3-methylimidazolium tetrafluoroborate and glacial acetic acid into a container at a ratio of 5:1:0.1, stir evenly, make the water phase and the ionic liquid miscible, and become a homogeneous phase, as Chicken sulfa drug residue extract.

[0062] (2) High-speed dispersion

[0063] Heat 6mL of the extract obtained in step (1) to a temperature of 30-40°C, add it to about 2 grams of chicken, and then use a high-speed disperser at 4000-8000rpm (preferably 5000-7000rpm) to disperse for 60-90s, and vortex After ultrasonic extraction for 3 minute...

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