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Method for detecting residual quantity of sulfonamides in swine urine

A technology of sulfonamides and residues, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as low detection limit

Inactive Publication Date: 2020-05-12
INST OF AGRI PROD QUALITY SAFETY & STANDARD JIANGXI ACAD OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0031] (3) Low detection limit in complex and dirty matrices

Method used

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  • Method for detecting residual quantity of sulfonamides in swine urine
  • Method for detecting residual quantity of sulfonamides in swine urine
  • Method for detecting residual quantity of sulfonamides in swine urine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0081] Draw 5.00mL sample, place it in a 50mL centrifuge tube, add 5g of anhydrous sodium sulfate and 15mL of acetonitrile solution, ultrasonically extract for 3min, and centrifuge at 5000r / min for 5min. Pour the supernatant into another centrifuge tube, add 15 mL of acetonitrile to the residue, and repeat the above operation once. The combined extracts were blown to nearly dry under nitrogen at 50°C, and 1.00 mL of dissolved residue was added accurately, filtered through a 0.22 μm filter membrane, and then determined by liquid chromatography-tandem mass spectrometer.

[0082] Set the liquid chromatography conditions as:

[0083] Chromatographic column: Eclipse Plus C18 (RRHD 1.8 μm, 2.1×100 mm). Mobile phase A is 0.1% formic acid aqueous solution; B is acetonitrile. Gradient elution program: 0~3.0min, 3%~8%B; 3.0~7.0min, 8%~90%B; 7.0~7.1min, 90%B~3%B; 7.1~9.0min, maintain 3% b. Flow rate 0.20mL / min; column temperature 30°C; injection volume: 5.0μL;

[0084] Mass Spectrom...

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Abstract

The invention relates to a method for detecting the residual quantity of sulfonamides in swine urine by ultra-high performance liquid chromatography-electrospray tandem mass spectrometry. The method comprises the following steps: sucking 5.00 mL of a sample, placing the sample in a 50 mL centrifuge tube, adding 5 g of anhydrous sodium sulfate and 15 mL of an acetonitrile solution, carrying out ultrasonic extraction for 3 min, and centrifuging at 5000 r / min for 5 min; pouring the supernatant into another centrifuge tube, adding 15 mL of acetonitrile into the residue, and repeating the operationonce. Mixing extracting solutions, blowing nitrogen to be nearly dry at 50 DEG C, accurately adding 1.00 mL of dissolved residues, filtering through a 0.22 mm filter membrane, and determining by using a liquid chromatography-tandem mass spectrometer.

Description

technical field [0001] The invention belongs to the field of drug residue detection, in particular to a method for qualitatively and quantitatively detecting sulfonamide drug residues in pig urine. Background technique [0002] Sulfa drugs (SAs) are a class of traditional synthetic antibacterial drugs, which have been widely used in veterinary clinics and animal husbandry because of their broad antibacterial spectrum, low price and easy availability. Thyroid hyperplasia or tumors in rodents, sulfa drugs are highly toxic, can destroy human hematopoietic function, and have a long residual half-life in food, which is significantly harmful to humans and the environment. Sulfonamide antibiotics are a kind of specific antibacterial drugs derived from p-aminobenzenesulfonamide as the basic structure. Although they play an important role in the treatment of human diseases, excessive use will cause toxic and side effects to the human body. The main manifestations are: Toxic damage, ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 胡丽芳范芳邱素艳赖艳李瑞丽
Owner INST OF AGRI PROD QUALITY SAFETY & STANDARD JIANGXI ACAD OF AGRI SCI
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