Method for detecting residual quantity of multiple alkaline drugs in animal derived food

Abstract

The invention relates to the fields of analytical chemistry and food safety, in particular to a method for detecting the residual quantity of multiple alkaline drugs in animal derived food. Based on the vortex mixed extracting of acetonitrile, isopropanol and citric acid buffer solutions, the purification of a hydrophilic polystyrene-divinylbenzene solid phase extraction column and a cation exchange solid phase extraction column and the liquid phase chromatography-mass spectra determination, the method can detect the residual quantity of multiple alkaline drugs in pork, pork liver, eggs, shrimps and milk, such as beta-receptor agonists,sulfonamides, benzodiazepines, nitroimidazoles, benzimidazoles and triphenylmethanes. The method has the advantages of simple operation, fast and accurate detection and high efficiency.

Description

technical field

[0001] The invention relates to the fields of analytical chemistry and food safety, in particular to a method for detecting residues of various basic drugs in animal-derived foods. Background technique

[0002] With the increase of people's demand for animal-derived food, veterinary drugs (including feed drug additives) have been widely used in animal husbandry in the past 20 years, and the problem of veterinary drug residues in animal-derived food has gradually become a social concern that people generally pay attention to. focus. At present, the illegal use of prohibited drugs, the abuse of antibacterial drugs and drug additives, etc. have been the main reasons for the excessive residues of veterinary drugs in animal-derived foods in my country and the safety problems of livestock and poultry products. Drug residues can directly cause acute and chronic poisoning, allergies, and allergies to the human body, and indirectly cause potential harm to the human b...

Examples

Embodiment 1

[0047] Sample preparation and determination methods for 76 veterinary drug residues in pork:

[0048] (1) Accurately weigh 5g (accurate to 0.01g) uniform sample, add 30mL acetonitrile, 2mL isopropanol and 10mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 6mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL by rotation, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min a...

Embodiment 2

[0072] Sample preparation and determination method for 76 kinds of veterinary drug residues in pig liver:

[0073] (1) Accurately weigh 2g (accurate to 0.01g) uniform sample, add 15mL acetonitrile, 1mL isopropanol and 5mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 3mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min a...

Embodiment 3

[0080] Sample preparation and determination methods for 76 veterinary drug residues in eggs:

[0081] (1) Accurately weigh 2g (accurate to 0.01g) uniform sample, add 15mL acetonitrile, 1mL isopropanol and 5mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 3mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min at 4°C, and pa...

technical field

[0001] The invention relates to the fields of analytical chemistry and food safety, in particular to a method for detecting residues of various basic drugs in animal-derived foods. Background technique

[0002] With the increase of people's demand for animal-derived food, veterinary drugs (including feed drug additives) have been widely used in animal husbandry in the past 20 years, and the problem of veterinary drug residues in animal-derived food has gradually become a social concern that people generally pay attention to. focus. At present, the illegal use of prohibited drugs, the abuse of antibacterial drugs and drug additives, etc. have been the main reasons for the excessive residues of veterinary drugs in animal-derived foods in my country and the safety problems of livestock and poultry products. Drug residues can directly cause acute and chronic poisoning, allergies, and allergies to the human body, and indirectly cause potential harm to the human b...

Examples

Embodiment 1

[0047] Sample preparation and determination methods for 76 veterinary drug residues in pork:

[0048] (1) Accurately weigh 5g (accurate to 0.01g) uniform sample, add 30mL acetonitrile, 2mL isopropanol and 10mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 6mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL by rotation, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min a...

Embodiment 2

[0072] Sample preparation and determination method for 76 kinds of veterinary drug residues in pig liver:

[0073] (1) Accurately weigh 2g (accurate to 0.01g) uniform sample, add 15mL acetonitrile, 1mL isopropanol and 5mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 3mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min a...

Embodiment 3

[0080] Sample preparation and determination methods for 76 veterinary drug residues in eggs:

[0081] (1) Accurately weigh 2g (accurate to 0.01g) uniform sample, add 15mL acetonitrile, 1mL isopropanol and 5mL citric acid buffer solution (pH=2.5, weigh 10.5g citric acid monohydrate) into a 50mL plastic centrifuge tube (C 6 h 8 o 7 .H 2 O) and 10.2g magnesium chloride hexahydrate (MgCl 2 .6H 2 (0) Dissolve in 450mL water, adjust the pH to 2.5 with ammonia water, dilute with water to 500mL), vortex and extract at 2000r / min for 5min, centrifuge at 4000r / min for 5min, and transfer the supernatant to a 250mL pear-shaped bottle. Repeat the above extraction operation, combine the extracts, add 3mL of isopropanol, and concentrate at a temperature of 40±2°C to about 5mL, transfer the concentrate to a 50mL plastic centrifuge tube, and rinse the pear-shaped bottle with 5mL of citric acid buffer , combined washings, refrigerated centrifugation at 8,500 r / min for 10 min at 4°C, and pa...

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