Method for enriching nature tetracycline antibiotics in aquatic products

Abstract

The present invention discloses a method for enriching nature tetracycline antibiotics in aquatic products, and relates to a sample pretreatment in the field of food safety analysis. The method comprises the following steps: a 0.1 mol / L disodium ethylenediaminetetraacetate / Mcllvaine extraction buffer solution pretreatment, phenol or benzoic acid-modified polystyrene superparamagnetic bead adsorption, elution collection and the like, wherein an eluent can be directly added to liquid chromatography or LC-MS to carry out analysis. Compared with the traditional sample pretreatment method for tetracycline antibiotics in aquatic products, the method of the present invention has the following characteristics that: a sample pretreatment operation process is substantially simplified, a sample pretreatment time is shortened, the adsorbent use amount is reduced, and an extraction yield of the tetracycline antibiotics in the sample is increased.

Description

technical field

[0001] The invention relates to the field of food safety analysis, in particular to a magnetic dispersion solid-phase extraction method for enriching natural tetracycline antibiotics in aquatic products by using polystyrene magnetic spheres modified with phenol or benzoic acid functional groups on the surface. Background technique

[0002] Tetracyclines (Tetracyclines, TCs) are a class of broad-spectrum antibiotics produced by actinomycetes, which are divided into natural products (chlortetracycline, oxytetracycline, tetracycline and doxycycline) and semi-synthetic products (doxycycline, Methacycline, minocycline, and guanidine tetracycline, etc.) Chemical structure of the tetracycline family:

[0003]

[0004] Tetracycline, oxytetracycline, chlortetracycline and doxycycline are widely used in the prevention, treatment and growth promotion of aquatic diseases in aquaculture because of their excellent antibacterial properties, stable drug properties and lo...

Examples

Embodiment 1

[0029] Example 1 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 70 nm)

[0030] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.5% SDS 3 In the solution, 300 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 20 min, add 0.5 g of p-vinylphenol ...

Embodiment 2

[0031] Example 2 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 100 nm)

[0032] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.4% SDS 3 In the solution, 250 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 10 min, add 0.5 g of p-vinylphenol...

Embodiment 3

[0033] Example 3 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 200 nm)

[0034] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.3% SDS 3 In the solution, 200 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 10 min, add 0.5 g of p-vinylphenol...

technical field

[0001] The invention relates to the field of food safety analysis, in particular to a magnetic dispersion solid-phase extraction method for enriching natural tetracycline antibiotics in aquatic products by using polystyrene magnetic spheres modified with phenol or benzoic acid functional groups on the surface. Background technique

[0002] Tetracyclines (Tetracyclines, TCs) are a class of broad-spectrum antibiotics produced by actinomycetes, which are divided into natural products (chlortetracycline, oxytetracycline, tetracycline and doxycycline) and semi-synthetic products (doxycycline, Methacycline, minocycline, and guanidine tetracycline, etc.) Chemical structure of the tetracycline family:

[0003]

[0004] Tetracycline, oxytetracycline, chlortetracycline and doxycycline are widely used in the prevention, treatment and growth promotion of aquatic diseases in aquaculture because of their excellent antibacterial properties, stable drug properties and lo...

Examples

Embodiment 1

[0029] Example 1 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 70 nm)

[0030] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.5% SDS 3 In the solution, 300 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 20 min, add 0.5 g of p-vinylphenol ...

Embodiment 2

[0031] Example 2 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 100 nm)

[0032] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.4% SDS 3 In the solution, 250 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 10 min, add 0.5 g of p-vinylphenol...

Embodiment 3

[0033] Example 3 Synthesis of polystyrene magnetic spheres modified with phenol or benzoic acid functional groups (particle size: 200 nm)

[0034] Referring to the literature (Yan F, Li J, Zhang J, Liu F, Yang W. J. Nanopart. Res., 2009, 11(2):289~296), the chemical co-precipitation method was used to synthesize superparamagnetic Fe 3 o 4 nanoparticles, and Fe 3 o 4 The surface oil of the nanoparticles was acidified, washed with absolute ethanol and then blown dry with nitrogen; take 5 g of the surface oil acidified Fe 3 o 4 Nanoparticles, suspended Fe in 5 mL of styrene-hexadecane mixture with a volume ratio of 15:1 3 o 4 Nanoparticles, ultrasonic 5 min to form a magnetic fluid, transfer the magnetic fluid to 400 mL, 0.01M NaHCO containing 0.3% SDS 3 In the solution, 200 W (25KHz) power continued ultrasonic emulsification for 30 minutes to form a miniemulsion; add 0.1g K to the above miniemulsion 2 S 2 o 8 After reacting at 70°C for 10 min, add 0.5 g of p-vinylphenol...

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