Pretreatment method for detecting furazolidone metabolites in aquatic products

A technology for furazolidone and metabolites, which is applied in the field of pretreatment for the detection of furazolidone metabolites in aquatic products. It can solve the problems of long reaction time, long time consumption, and long processing time, so as to reduce reaction time, facilitate qualitative detection, and simplify The effect of the processing step

Inactive Publication Date: 2020-07-17
深圳市深大检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection steps in aquatic products are roughly divided into the following steps: cleaning to remove fat, hydrolysis and derivatization, purification and other steps. The reaction time in the process of hydrolysis and derivatization is relatively long, and the use of solid-phase extraction in the purification process requires a relatively high cost. A long time, in short, leads to a long pretreatment time when testing aquatic products

Method used

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  • Pretreatment method for detecting furazolidone metabolites in aquatic products
  • Pretreatment method for detecting furazolidone metabolites in aquatic products
  • Pretreatment method for detecting furazolidone metabolites in aquatic products

Examples

Experimental program
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Effect test

Embodiment 1

[0032] A pretreatment method for the detection of furazolidone metabolites in aquatic products, comprising the following steps:

[0033] S1: Grind the sample (the sample in this example is a shrimp meat sample) with a tissue grinder to obtain a sample;

[0034] S2: Weigh 5.00g sample and place it in a 50mL brown centrifuge tube, add 10mL of methanol and water mixed solution, the volume of methanol and water is 2:1, homogenize for 1min, rotate at 4000r / min, centrifuge for 5min, draw The supernatant was discarded, and the fat and free metabolites in the sample were removed to obtain material A;

[0035] S3: First add 0.20 g of sodium chloride to the material A in step 2, mix well, then add 10 mL of 0.5 mol / L hydrochloric acid solution, after mixing well, sonicate for 30 min, then add 200 μL of 2-hydroxy-1-naphthaldehyde solution, Shake well, and sonicate at 50°C for 2 hours to obtain material B;

[0036] S4: After the reaction is complete, add 10 mL of ethyl acetate to materia...

Embodiment 2

[0040] Embodiment 2 is identical with each raw material consumption of embodiment 1, and difference is the difference of process parameter in the reaction process, specifically:

[0041] S1: Grind the sample (the sample in this example is a shrimp meat sample) with a tissue grinder to obtain a sample;

[0042] S2: Weigh 5.00g sample and place it in a 50mL brown centrifuge tube, add 10mL of methanol and water mixed solution, the volume of methanol and water is 2:1, homogenize for 1min, rotate at 3000r / min, centrifuge for 7min, draw The supernatant was discarded, and the fat and free metabolites in the sample were removed to obtain material A;

[0043] S3: Add 0.20 g of sodium chloride to the material A in step 2, mix well, then add 10 mL of 0.5 mol / L hydrochloric acid solution, mix well, ultrasonicate for 30 min, then add 200 μL of 2-hydroxy-1-naphthaldehyde solution, shake Shake well, and sonicate at 55°C for 1.5h to obtain material B;

[0044] S4: After the reaction is comp...

Embodiment 3

[0048] Embodiment 3 is identical with each raw material consumption of embodiment 1, and difference is the difference of process parameter in the reaction process, specifically:

[0049]S1: Grind the sample (the sample in this example is a shrimp meat sample) with a tissue grinder to obtain a sample;

[0050] S2: Weigh 5.00g sample and place it in a 50mL brown centrifuge tube, add 10mL of methanol and water mixed solution, the volume of methanol and water is 2:1, homogenize for 1min, rotate at 2000r / min, centrifuge for 10min, draw The supernatant was discarded, and the fat and free metabolites in the sample were removed to obtain material A;

[0051] S3: Add 0.20g of sodium chloride to material A in step 2, mix well, then add 10mL of 0.5mol / L hydrochloric acid solution, mix well, ultrasonicate for 30min, then add 200μL of 2-hydroxy-1-naphthaldehyde solution , oscillate and shake well, and sonicate at 60°C for 1 hour to obtain material B;

[0052] S4: After the reaction is co...

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Abstract

The invention discloses a pretreatment method for detecting furazolidone metabolites in aquatic products. The pretreatment method comprises the steps of S1 crushing a sample to obtain a sample; S2 weighing a sample, adding a mixed solution of methanol and water, homogenizing, and removing fat in the sample to obtain a material A; S3 adding neutral salt, hydrochloric acid and a derivatization reagent into the material A, and performing ultrasonic treatment for 1 to 2 hours at the temperature of 50 to 60 DEG C to obtain a material B; S4 adding an extracting agent into the material B, carrying out ultrasonic treatment and centrifugation, and taking an upper-layer solution to obtain a material C; S5 carrying out secondary extraction by using an extracting agent, and combining the filtrate withthe material C to obtain a material D; S6 adding a dehydrating agent into the material D, filtering, taking filtrate, and volatilizing the extracting agent to obtain a to-be-detected substance. The method is capable of shortening the pretreatment time.

Description

technical field [0001] The invention relates to the technical field of furazolidone metabolite detection, more specifically, it relates to a pretreatment method for furazolidone metabolite detection in aquatic products. Background technique [0002] Furazolidone drugs are a kind of artificially synthesized spectrum antibiotics, which are widely used in the prevention and treatment of dysentery, enteritis and coccidiosis in livestock, poultry and aquatic products because of their low price and good use effect. Since the residues of furazolidone metabolites in animal-derived foods can be transmitted to humans through the food chain, long-term intake can cause carcinogenic, teratogenic and other side effects on the human body. Some countries have banned the use of furazolidone drugs in poultry and aquaculture. However, furazolidone metabolizes rapidly in vivo and cannot be detected. However, furazolidone metabolites are easy to bind to proteins to ensure long-term stable existe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/067G01N2030/062
Inventor 李清燕周清平
Owner 深圳市深大检测有限公司
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