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A pretreatment method for improving the measurement accuracy of sulfonamide drug residues in meat

A technology for sulfonamide drugs and accuracy is applied in the field of pretreatment to improve the accuracy of determination of sulfonamide drug residues in meat, and can solve problems such as easy bumping, time-consuming, affecting detection results, etc., so as to improve the recovery rate and improve the accuracy. degree of effect

Inactive Publication Date: 2018-06-26
PUBLIC MONITORING CENT FOR AGRO PROD OF GUANGDONG ACADEMY OF AGRI SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] After repeated research by the inventors, it was found that the reason why the qualified rate of sulfonamides is low is mainly that there is a defect in the concentration and purification link of the sample pretreatment.
In this method, the extract in the later stage of extraction needs to be concentrated to dryness, which is time-consuming and prone to bumping during the concentration process
The concentrated residue was redissolved with 3 mL of reconstitution solution acetonitrile-water (95+5). Due to the high water content in the reconstitution solution, the water content in the obtained reconstitution solution was greater than 5%, which lowered the recovery rate of the drug and affected Final test result

Method used

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  • A pretreatment method for improving the measurement accuracy of sulfonamide drug residues in meat
  • A pretreatment method for improving the measurement accuracy of sulfonamide drug residues in meat
  • A pretreatment method for improving the measurement accuracy of sulfonamide drug residues in meat

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Embodiment 1

[0032] (1) Extraction: Weigh 5±0.05 g of the sample into a polypropylene centrifuge tube, add 4 g of anhydrous sodium sulfate and 25 mL of acetonitrile, vortex and mix for 15 s, oscillate at a medium speed for 20 min, and centrifuge at 2500 r / min for 5 min, move the supernatant to a separatory funnel, add 30 mL of n-hexane, shake for 2 min, then stand still for 5 min, separate the acetonitrile layer, repeat the extraction once with 25 mL of acetonitrile, and wash the acetonitrile layer with the same n-hexane After partitioning with alkanes, combine the acetonitrile layer into a 100 mL heart-shaped bottle, add 5 mL of n-propanol, and concentrate under reduced pressure at 50°C to a volume of 300-600 μL to obtain a residue;

[0033](2) Purification: add acetonitrile to the residual solution to redissolve, and control the water content of the solution below 5%. ) to wash the chicken heart bottle, and pass through the basic alumina SPE column, blow off the liquid retained in the co...

Embodiment 2

[0038] (1) Extraction: Weigh 5±0.05g of the sample into a polypropylene centrifuge tube, add 4g of anhydrous sodium sulfate and 25mL of acetonitrile, vortex for 15s, oscillate at a medium speed for 20min, centrifuge at 2500r / min for 5min, and the supernatant Move to a separatory funnel, add 30mL of n-hexane, shake for 2min, stand still for 5min, separate the acetonitrile layer, repeat the extraction once with 25mL of acetonitrile, and divide the acetonitrile layer with the same part of n-hexane, combine the acetonitrile layer into 100mL chicken hearts Add 5 mL of n-propanol to the bottle, concentrate under reduced pressure at 50°C to a volume of 300-600 μL to obtain a residue;

[0039] (2) Purification: Add acetonitrile to the residual solution to redissolve, and control the water content of the solution below 5%. The obtained reconstituted solution is all perbasic alumina SPE column, not collected, and then mixed with 5mL acetonitrile-water (95+5) Wash the heart bottle, and p...

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Abstract

The invention provides a pretreatment method for improving accuracy of measuring sulfonamide residues in meat. The pretreatment method comprises the following step one of extraction, wherein a meat test sample is taken and extracted with acetonitrile twice, supernatant extracted twice is allocated with n-hexane, then acetonitrile layers are combined, 5 mL of n-propyl alcohol is added, the mixture is concentrated in a pressure reduction mode at the temperature of 50 DEG C until the size is 300-600 MuL, and residue liquid is obtained; the step two of purification, wherein acetonitrile is added to the residue liquid for redissolving, the water content in the solution is controlled to be 5% or below, an obtained compound solution is totally subjected to the alkaline aluminum oxide SPE column, acetonitrile-water is used for elution, eluant is collected and filtered to obtain a test sample solution, and the test sample solution is measured through high-performance liquid chromatography. The method is simple and easy to operate, and can improve the accuracy for measuring the sulfonamide residues through the high-performance liquid chromatography.

Description

technical field [0001] The invention relates to a method for measuring sulfa drug residues in meat, in particular to a pretreatment method for improving the accuracy of measuring sulfa drug residues in meat. Background technique [0002] Sulfonamides (sulfanilamides, SAs) are structurally similar to p-aminobenzoic acid (PABA), which can compete with PABA to act on the dihydrofolate synthase in bacteria, thereby preventing the synthesis of tetrahydrofolate required by bacteria using PABA as a raw material. And then inhibit the synthesis of bacterial protein to achieve antibacterial effect. These drugs have broad antibacterial spectrum, obvious antibacterial effect, stable properties and low price, so they are widely used in the prevention and treatment of bacterial infection diseases in livestock and poultry. However, sulfonamides cannot be completely metabolized in animals, and their residues can enter the human body through the food chain, thereby posing a threat to human ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/14G01N30/02
CPCG01N30/02G01N30/14G01N2030/027
Inventor 殷秋妙吴维煇王威利林雪贤张展续倩李亚菲
Owner PUBLIC MONITORING CENT FOR AGRO PROD OF GUANGDONG ACADEMY OF AGRI SCI
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