Measuring method for nitrofuran medicines in pork

Abstract

The invention discloses a measuring method for nitrofuran medicines in pork. The measuring method comprises the following steps that: (1) adding a homogeneous pork sample into a centrifuge tube, adding mixed solvent of water and methyl alcohol to carry out vortex mixing and centrifugation to obtain solid sediments; (2) adding interior standard liquid into the solid sediments of S(1), evenly mixing, an adding acidic reagent and deriving agent to carry out deriving processing; (3) regulating the pH (Potential of Hydrogen) value of the derived solution of S(2) to be neutral, adding normal hexaneto evenly shake and carry out centrifugation, adding clear solution in a salt packet tube, and carrying out centrifugation by acetonitrile and formic acid aqueous solution in sequence to obtain extracting solution; and (4) filtering the extracting solution, and carrying out computer testing on filtrate. By use of the measuring method disclosed by the invention, a sample does not need to be processed by a solid phase extraction column, a step of extracting and drying by blowing through ethyl acetate is not required, preliminary treatment is simple and convenient, preliminary treatment time is shortened, detection efficiency is improved, and in addition, detection data obtained by the method is stable and reliable.

Description

technical field

[0001] The invention relates to a detection method of organic compounds in food, more specifically, to a detection method of nitrofuran drugs in pork. Background technique

[0002] Pork, also known as porridge, is the meat of one of the main domestic animals, the pig family pig. Its nature and taste are sweet and flat, rich in protein and fat, carbohydrates, calcium, iron, phosphorus and other nutrients. Pork is the main non-staple food in daily life. It has the functions of tonifying deficiency and strengthening the body, nourishing yin and moistening dryness, and plumping the skin. Anyone who is weak after illness, postpartum blood deficiency, yellow and thin, can be used as a nourishing product.

[0003] Therefore, in order to ensure the safety of pork and meet the detection requirements, it is very important to establish a detection method that can accurately and efficiently determine nitrofurans in pork. In the prior art, most of the pork is processed...

Examples

Embodiment 1

[0022] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0023] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 4750r / min for 10min. Remove 6.50mL of supernatant, put it into a salt-packed tube containin...

Embodiment 2

[0025] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0026] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 5000r / min for 8min. Remove 6.50mL of supernatant, put it into a salt-packed tube containing...

Embodiment 3

[0028] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0029] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 4500r / min for 10min. Remove 6.50mL of supernatant, put it into a salt-packed tube containin...

technical field

[0001] The invention relates to a detection method of organic compounds in food, more specifically, to a detection method of nitrofuran drugs in pork. Background technique

[0002] Pork, also known as porridge, is the meat of one of the main domestic animals, the pig family pig. Its nature and taste are sweet and flat, rich in protein and fat, carbohydrates, calcium, iron, phosphorus and other nutrients. Pork is the main non-staple food in daily life. It has the functions of tonifying deficiency and strengthening the body, nourishing yin and moistening dryness, and plumping the skin. Anyone who is weak after illness, postpartum blood deficiency, yellow and thin, can be used as a nourishing product.

[0003] Therefore, in order to ensure the safety of pork and meet the detection requirements, it is very important to establish a detection method that can accurately and efficiently determine nitrofurans in pork. In the prior art, most of the pork is processed...

Examples

Embodiment 1

[0022] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0023] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 4750r / min for 10min. Remove 6.50mL of supernatant, put it into a salt-packed tube containin...

Embodiment 2

[0025] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0026] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 5000r / min for 8min. Remove 6.50mL of supernatant, put it into a salt-packed tube containing...

Embodiment 3

[0028] Weigh 2.00g of homogeneous pork sample into a 50mL centrifuge tube, add 10mL of methanol and water mixed solvent (the volume ratio of methanol to water is 1:1), vortex for 10min, centrifuge at 4750r / min for 5min, discard A solid precipitate was obtained from the supernatant, and 100 μL of internal standard solution was added to the solid precipitate, followed by 10 mL of hydrochloric acid solution and 100 μL of o-nitrobenzaldehyde derivative, vortexed for 10 min, and placed in a 37°C water bath for 16 h.

[0029] Take out the solution, put it at room temperature, add 10mL hydrochloric acid solution to the blank centrifuge tube in advance, then add the solution, 2mL phosphate buffer, add sodium hydroxide solution one by one, measure the pH value after each addition of sodium hydroxide solution, and adjust to pH 7.4, shake gently, add 15mL of n-hexane, shake well, and centrifuge at 4500r / min for 10min. Remove 6.50mL of supernatant, put it into a salt-packed tube containin...

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