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Compound detection reagent for detecting sulfonamide compound and detection method thereof

A combination of detection and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large sample matrix interference, cumbersome methods, and difficult qualitative confirmation, and achieve low false negative and false positive rates and a wide range of detection , Eliminate the effect of matrix effect

Active Publication Date: 2016-10-12
吕晶
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Enzyme-linked immunoassay and radioimmunoassay are mainly used for large-scale screening work, which are prone to false positives, and are generally not used for quantification; gas chromatography uses electron capture detector for quantitative analysis, which has high specificity, but this method is relatively It is cumbersome and difficult to operate; high performance liquid chromatography ultraviolet detection and capillary electrophoresis have low sensitivity and poor specificity, especially when the sample matrix interferes with low concentration detection, it is difficult to accurately confirm qualitatively; although gas chromatography-mass spectrometry is sensitive and specific High stability, but the derivatization process is cumbersome, not suitable for high-throughput analysis

Method used

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  • Compound detection reagent for detecting sulfonamide compound and detection method thereof
  • Compound detection reagent for detecting sulfonamide compound and detection method thereof
  • Compound detection reagent for detecting sulfonamide compound and detection method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1. Experimental instruments and reagents

[0031] 1.1 Experimental Instruments

[0032] AcQuity TM UPLC ultra-high pressure liquid chromatography, Oasis MCX solid phase extraction (SPE) cartridge (3ml, 60mg) were purchased from Waters, USA, API5500Qtrap mass spectrometer was purchased from AB, USA, vortex mixer, TTL-DC II nitrogen blowing instrument, IKA High-speed tissue homogenizer, ultrapure water instrument (Simplicity, Merck Millipore), ultrasonic extractor (KQ-250B, Kunshan Ultrasonic Instrument Co., Ltd.), IKA T18Basic high-speed disperser (Germany).

[0033] 1.2 Experimental reagents

[0034] Methanol (chromatographically pure), acetonitrile (chromatographically pure) formic acid has a purity of 99%, 28 kinds of sulfa compounds (purity ≥ 99%): sulfamerazine, sulfamethoxazine, sulfachloropyridazine, sulfabenzoyl, sulfamethoxazole Soxin, sulfaquinoxaline, sulfabenzopyrazole, sulfanitrobenzene, sulfadiazine, sulfacetamide, sulfapyridine, sulfathiazole, sulfamet...

Embodiment 2

[0064] Embodiment 2, the specific detection and analysis of the sample to be detected

[0065] The actual samples to be tested were purchased from the market in Shandong Province. After processing, they were stored in a refrigerator at 4°C for later use. 10 parts of duck samples purchased are detected by the detection method of the present invention, and 1 routine positive sample is found, and it is detected that the sulfanitrobenzene content is 0.52ng / mL, see figure 2 .

[0066] The concrete detection method of this embodiment is as follows:

[0067] (1) Biological sample pretreatment: the pretreatment in this embodiment adopts the protein precipitation method (using the protein precipitation agent in the combined detection reagent) for treatment. Select the duck meat sample, cut it into pieces, remove the fascia, accurately weigh 1.00g of the duck meat sample, add 3mL of water, and evenly mash it with a high-speed tissue disperser to make a homogenate sample, accurately w...

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Abstract

The invention provides a compound detection reagent for detecting a sulfonamide compound and a detection method thereof. The compound detection reagent is prepared from an organic solvent solution containing various sulfonamide compound reference substances and a protein precipitator. The compound detection reagent provided by the invention can be used for simultaneously analyzing and detecting 28 sulfonamide compounds; the detection scope is wide; the scheme of protein precipitation or liquid-liquid extraction is adopted in the process of sample treatment, so that 28 sulfonamide compounds in the biological sample are purified and enriched; the detection method adopting the compound detection reagent provided by the invention has the advantages of simplicity, accuracy, quickness, stability and less sample capacity; the complex steps of derivatization and enzymatic conversion are not required; the chemical reagent used in the pre-treating process is less; the detection method is environment-friendly; the detection result is not interfered by endogenous substances; the false negative / positive rate is low; the cost of the reagent is low; the compound detection reagent is fit for quick analysis for a large amount of samples.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a combined detection reagent for detecting sulfonamide compounds and a detection method thereof. Background technique [0002] Sulfonamides (SAs) refer to the general term for a class of drugs with the structure of sulfanilamide, which have the advantages of broad antibacterial spectrum and strong curative effect, and are one of the most commonly used antibiotics in the aquaculture industry. Due to the long action and metabolism time of SAs in the body, sulfonamides ingested through any route may accumulate in the human body, and when the concentration exceeds a certain value, it will cause harm to human body functions. The toxic effects of SAs drugs are mainly reflected in kidney damage, tumorigenic effect, allergic reaction, hematopoietic function destruction, and digestive system disorders. Because sulfonamides are more harmful and are widely used in farmin...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 李鹰飞
Owner 吕晶
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