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Analyzing method of residues of sulfanilamide and antibiotic medicaments in aquatic product

An analytical method and antibiotic technology, applied in the direction of analytical materials, preparation of test samples, material separation, etc., can solve problems such as time-consuming and laborious, and achieve the effects of short analysis time, pollution reduction, and environmental friendliness.

Inactive Publication Date: 2010-02-03
赖克强 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing detection methods can only detect the above two categories of drugs separately, which is time-consuming and labor-intensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 1.0g of fish meat with a spiked concentration of 0.10ppm and mix it uniformly in a glass mortar, add 1.0g of methanol-treated C18 filler and 0.5g of EDTA sodium salt, and grind it with a glass pestle for about 5 minutes to mix the fish and filler evenly . Remove the 10mL syringe with the membrane gasket at the end, load the sample into the column, and press it gently with filter paper. Wash once with 10 mL of n-hexane (60 drops at a flow rate of 1 min), and dry in vacuum (discard the eluent); then elute with 10 mL of acetonitrile (60 drops at a flow rate of 1 min), and dry in a vacuum. The eluate was evaporated to near dryness at 35°C, then dried with air flow, and then 2 mL of 40% (volume ratio) methanol aqueous solution was added to dissolve the residue, passed through a 0.45 μm filter membrane, and then determined by HPLC. Use oxalic acid-methanol buffer solution as mobile phase, pH is about 3.0; Gradient elution: 0~5min 80:20 (V / V, volume ratio), 6~20min 75:2...

Embodiment 2

[0038]Weigh 1.0g of shrimp meat with a spiked concentration of 0.20ppm and mix it uniformly in a glass mortar, add 1.0g of methanol-treated C18 filler and 0.5g of EDTA sodium salt, and grind it with a glass pestle for about 5min to make the shrimp meat and filler well mixed. Remove the 10mL syringe with the membrane gasket at the end, load the sample into the column, and press it gently with filter paper. Wash once with 10 mL of n-hexane (60 drops at a flow rate of 1 min), and dry in a vacuum (discard the eluent); then elute with 5 mL of methanol and 5 mL of acetonitrile (60 drops at a flow rate of 1 min), and dry in a vacuum. The eluate was evaporated to near dryness at 35°C, then dried with air flow, and then 2 mL of 40% (volume ratio) methanol aqueous solution was added to dissolve the residue, passed through a 0.45 μm filter membrane, and then determined by HPLC. Use oxalic acid-methanol buffer solution as mobile phase, pH is about 3.0; Gradient elution: 0~5min 80:20 (V / V...

Embodiment 3

[0040] Weigh 1.0 g of crab meat with a spiked concentration of 0.50 ppm and mix it uniformly in a glass mortar, add 1.0 g of methanol-treated C18 filler and 0.5 g of EDTA sodium salt, and grind it with a glass pestle for about 5 minutes to make the crab meat and filler well mixed. Remove the 10mL syringe with the membrane gasket at the end, load the sample into the column, and press it gently with filter paper. Wash once with 10 mL of n-hexane (60 drops at a flow rate of 1 min), and dry in a vacuum (discard the eluent); then elute with a mixed solution of 10 mL of oxalic acid and acetonitrile (60 drops at a flow rate of 1 min), and dry in a vacuum. The eluate was evaporated to near dryness at 35°C, then dried with air flow, and then 2 mL of 40% (volume ratio) methanol aqueous solution was added to dissolve the residue, passed through a 0.45 μm filter membrane, and then determined by HPLC. Use oxalic acid-methanol buffer solution as mobile phase, pH is about 3.0; Gradient elut...

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Abstract

The invention relates to a detection method of residues in tissue of an aquatic product, in particular to an analyzing method of residues of sulfanilamide and antibiotic medicaments in an aquatic product, which comprises the following steps: adding filler and EDTA sodium salt to the tissue of an aquatic product to be detected and mixing the components to obtain a mixed material; drip washing the mixed material by a drip washing agent; eluting the obtained mixed material by an eluting agent to obtain an eluant; concentrating the eluant obtained in the eluting step, dissolving the concentrated eluant by a solvent and then filtering the eluant to obtain a filter liquor; and using a buffer solution as a flowing phase to carry out HPLC measurement on the filter liquor. The method can simultaneously detect the residues of sulfanilamide and tetracycline medicaments in a sample to be detected.

Description

technical field [0001] The invention relates to a detection method for residues in aquatic product tissues, in particular to an analysis method for multiple residues of sulfonamides and antibiotics in aquatic products. Background technique [0002] Sulfonamides and tetracyclines, as broad-spectrum antimicrobials, are widely used as additives in aquaculture to prevent intestinal infection and promote growth. However, if it is used improperly, it will cause problems such as toxic reactions, double infection, and bacterial drug resistance, causing direct or potential harm to food safety, the ecological environment, and human health. research focus. At present, there are many domestic and foreign reports on multi-residue detection techniques of sulfonamides and tetracyclines in aquatic products, mainly including high performance liquid chromatography, capillary zone electrophoresis, gas chromatography, liquid chromatography-mass spectrometry, etc., but the methods used The met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/28G01N1/34G01N1/44G01N30/36
Inventor 赖克强俞志根陆勤丰丛健
Owner 赖克强
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