Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof

A two-phase system and ionic liquid technology, which is applied in solvent extraction, preparation of test samples, separation methods, etc., can solve the problems of no description or disclosure of the amount of ionic liquid and inorganic salt and their proportional relationship

Inactive Publication Date: 2009-08-12
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the application does not describe or disclose the specific amount and proportion of the ionic liquid and inorganic salt used.

Method used

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  • Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof
  • Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof
  • Ionic liquid double-aqueous phase system for extracting residual antibiotic in foodstuffs and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] The synthesis of embodiment 1 ionic liquid

[0088] Add 0.1mol of pyridine, 0.1mol of bromoethane and 15mL of cyclohexane to a 50mL two-necked flask in sequence, and stir and reflux at 30-40°C for over 24hr. The resulting product is recrystallized several times with absolute ethanol and ethyl acetate to obtain white crystals, which are alkyl-substituted pyridinium ions ([RPy] + ), the product purity is greater than 98%. The product has passed FT-IR, 1 H-NMR and 13 C-NMR characterization.

[0089] According to the above-mentioned same preparation method, use raw material 2-picoline or 4-picoline instead of pyridine to obtain alkyl-substituted 2-picoline ion ([R, 2-MPy] + ) or alkyl-substituted 4-methylpyridinium ion ([R, 4-MPy] + ).

Embodiment 2

[0090] The detection of chloramphenicol in embodiment 2 eggs

[0091] Pretreatment of egg samples:

[0092]Accurately weigh 5 g of broken egg liquid into a 25 ml centrifuge tube, add 0.05 μg of chloramphenicol (the content of chloramphenicol is 10 μg / kg broken egg liquid), then add pH 7.0, NaCl concentration of 40 g / L phosphate buffer and mix Extraction solution 3ml, which contains methanol 100μl. Vortex to mix and then centrifuge at a speed of 10,000r / min. After centrifugation, transfer the supernatant to another centrifuge tube, and then add 3ml of the above-mentioned mixed extraction solution to the lower layer. After repeating the above operation, combine the supernatant and blow off the methanol. stand still. Add 3ml of n-hexane, vibrate and centrifuge, repeat the operation 2-3 times, discard the upper layer, and dilute to 5ml with ultrapure water to prepare an egg standard sample solution, a broken egg sample solution with a chloramphenicol content of 10 μg / kg.

[009...

Embodiment 3

[0097] Example 3 Detection of Chloramphenicol in Eggs

[0098] According to the same method as in Example 2, the egg sample liquid to be tested with a chloramphenicol content of 20 μg / kg, 40 μg / kg and 200 μg / kg was obtained, and the same ionic liquid-inorganic salt and detection method as in Example 2 were used for detection. .

[0099] Through analysis and calculation (that is, on the standard curve with the concentration as the abscissa and the peak area as the ordinate, the corresponding sample concentration is determined according to the measured peak area), and the analysis and detection results of the four concentrations are shown in Table 1.

[0100] Table 1 Determination results of chloramphenicol in egg samples

[0101]

[0102] Ionic liquid ethylpyridine bromide ([EPy]Br) and K 2 HPO 4 The extraction rate of chloramphenicol in the broken egg liquid is greater than 90%.

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Abstract

An ionic liquid dual aqueous phase system for extracting residual antibiotics in food is disclosed. The dual aqueous phase system formed by ionic liquid and inorganic salt realizes efficient extraction of residual antibiotics in food. Specific pyridine ionic liquid and specific inorganic salt are mixed according to the proportion of 1-20% (w / v) ionic liquid and 40-56% (w / v) of inorganic salt to ensure the extraction rate of antibiotics in food by the ionic liquid dual aqueous phase system to be larger than or equal to 90%, thus remarkably improving the sensitivity and reliability of detection of antibiotics residual in food.

Description

technical field [0001] The present invention relates to an ionic liquid two-water phase, in particular to an ionic liquid-inorganic salt two-water system, more specifically to an ionic liquid two-water system for extracting residual antibiotics in food and its application in the detection of antibiotic residues Applications. Background technique [0002] With the large-scale development of the aquaculture industry, veterinary drugs are widely used in the aquaculture industry to prevent and treat animal diseases, and at the same time there is a tendency to abuse them. In terms of detection technology for banned veterinary drugs, my country currently only has national standards for clenbuterol hydrochloride (GC-MS method) and diethylstilbestrol (HPLC-UV detection); the Ministry of Agriculture has announced detection methods for 10 types of drugs, of which only nitroimidazole (liquid chromatography) and chloramphenicol (liquid chromatography) are banned drugs; 16 banned drugs r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/00G01N1/32G01N1/40
Inventor 李蕾赵第海曾延波邹建军
Owner JIAXING UNIV
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