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Determination method of residual quantity of five sulfonamides in animal foods

A technology for sulfonamide drugs and animal food, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of time-consuming, inability to automate, complicated steps, etc., and achieve high extraction efficiency, good recovery rate and repeatability, and easy operation. simple effect

Inactive Publication Date: 2011-06-01
BEIJING JITIAN INSTR CO LTD
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  • Description
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Problems solved by technology

Chinese invention patent CN 100376893C discloses a liquid chromatography method for determining sulfamethoxazole in fish meat. During the sample pretreatment of the method, the sample will be mixed with hydrochloric acid and left for 1 hour, and then mixed with dihydrochloric acid in a ratio of 3:1. Methyl chloride / acetone mixture is used as the extraction solution. After adding the extraction solution, it still needs to stand in a refrigerator at 4°C for 8-12 hours. It also needs to be homogenized with a high-speed homogenizer and centrifuged multiple times. The steps are complicated and time-consuming. cannot be automated

Method used

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  • Determination method of residual quantity of five sulfonamides in animal foods
  • Determination method of residual quantity of five sulfonamides in animal foods
  • Determination method of residual quantity of five sulfonamides in animal foods

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Embodiment 1

[0023] Measure 5 chicken samples, mince the samples, and store them frozen at -18°C;

[0024] Sample pretreatment: Accurately weigh 1g of sample, mix it with 2g of diatomaceous earth until the sample has no agglomeration, transfer it to the extraction pool with a layer of fiber filter paper at the bottom, place the extraction pool on a fast solvent extractor for extraction, and extract Solvent: acetonitrile, temperature: 120°C, pressure: 10.0MPa, heating time: 5min, static time: 5min, flushing volume: 40% of the volume of the extraction cell, nitrogen purge time: 60s, static cycle times: 1 time, with acetonitrile Rinse the sample quickly, and collect all the extract by nitrogen purge. Add 5ml of n-hexane to the obtained extract to remove lipid impurities, vibrate vigorously and then separate into layers, discard the n-hexane layer, then add 5ml of n-hexane to repeat the operation twice, transfer the lower layer solution into a concentrated bottle, and place in a water bath at ...

Embodiment 2

[0037] Measure 5 beef samples, mince the samples, and store them frozen at -18°C;

[0038] Sample pretreatment: Accurately weigh 1g of sample, mix it with 3g of diatomaceous earth until the sample has no agglomeration, transfer it to the extraction pool with a layer of fiber filter paper at the bottom, place the extraction pool on a fast solvent extraction instrument for extraction, and extract Solvent: acetonitrile, temperature: 120°C, pressure: 10.0MPa, heating time: 5min, static time: 5min, flushing volume: 40% of the volume of the extraction cell, nitrogen purge time: 60s, static cycle times: 1 time, with acetonitrile Rinse the sample quickly and collect all the extract by nitrogen purge. Add 5ml / g n-hexane to the obtained extract to remove lipid impurities, vibrate vigorously and then separate into layers, discard the n-hexane layer, then add 5ml n-hexane to repeat the operation twice, transfer the lower layer solution into a concentrated bottle, and place in a water bath...

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Abstract

The invention relates to a determination method of residual quantity of five sulfonamides in animal foods, in particular to a liquid-phase chromatography method for determining the drug residual quantity in the animal foods, aiming to provide a determination method which has the advantages of simple operation, rapidness, high automation degree, high extraction efficiency, good recovery rate and good repeatability. The determination method of the residual quantity of the five sulfonamides in the animal foods comprises the following steps of sample preparation; sample pre-treatment: weighing a sample, uniformly mixing the sample with diatomite, transferring the mixture into an extraction pool, arranging the extraction pool on a rapid solvent extraction apparatus to extract, adding n-hexane in the obtained extract to remove lipid impurities, violently oscillating, standing for layering, removing an n-hexane layer, adding the n-hexane again to repeat the operation twice, transferring a solution at the lower layer into a concentration bottle, carrying out reduced pressure distillation on the solution in a rotary evaporimeter until dry, dissolving residual slags with a mobile phase, filtering the solution with a filter membrane, and analyzing with HPLC (High-Efficiency Liquid-Phase Chromatography); standard solution preparation; and high-efficiency liquid-phase chromatographic determination.

Description

technical field [0001] The invention relates to a method for determining the residual amount of veterinary drugs in animal food, in particular to a method for determining sulfadiazine, sulfamethazine, sulfamethazine, sulfamethoxazole and sulfadimethoxy in animal food Liquid Chromatography for the Residues of Five Sulfonamides in Pyrimidine. Background technique [0002] Sulfonamides are widely used in animal husbandry and play a significant role in reducing animal morbidity and mortality; they can also significantly improve the quality of aquatic animals. However, if long-term consumption of animal food containing sulfonamide drug residues, the residual drugs can cause poisoning; damage the human hematopoietic system, causing hemolytic anemia, agranulocytosis, thrombocytopenia and other diseases; and even affect the central nervous system. The residues of sulfa drugs not only bring great harm to human health, but also seriously affect the export of animal food in my country...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 于辉赵萍
Owner BEIJING JITIAN INSTR CO LTD
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