Method for detecting sulfonamide residue in eel by pressurized capillary electrochromatography
A technology of capillary electrochromatography and sulfonamide drugs, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor detection sensitivity and specificity, small amount of capillary electrophoresis sample injection, and inability to measure residues, etc., to achieve increased sensitivity, Meet the needs of daily detection of sulfa drugs, reduce the content of impurities and the effect of matrix interference
Inactive Publication Date: 2013-03-06
ZHEJIANG OCEAN UNIV
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These methods have different advantages and disadvantages: the detection speed of microbiological method is fast, but the detection sensitivity and specificity are poor; the sensitivity and selectivity of thin layer chromatography are good, but the repeatability is not good enough; the biggest deficiency of capillary
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[0025] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
[0026] 1 Sample preparation: Cut the eel muscle tissue samples into pieces with scissors, homogenize them with a high-speed homogenizer, and store them in a freezer.
[0027] 2 Sample pretreatment:
[0028] (1) Extraction: Thaw the sample, accurately weigh 5g (accurate to 0.01g) of homogeneous sample and place it in a 50mL centrifuge tube, add 5g of dry anhydrous sodium sulfate and 15mL of ethyl acetate, and mix thoroughly with a vortex mixer Homogenize for 2 minutes, centrifuge at 5000r / min for 10 minutes, transfer the supernatant to a 100mL separatory funnel, then add 15mL ethyl acetate to the original centrifuge tube to repeat the extraction once, combine the two supernatants into the separatory funnel, add 15mL n-hexane Alkanes, oscillate to make it fully mixed, let stand, discard the n-hexane layer, transfer the ethyl acetate layer to a ...
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Abstract
The invention relates to a method for detecting sulfonamide residues in eel by pressurized capillary electrochromatography, which is characterized in that the method comprises the following steps: extracting a sample by ethyl acetate, purifying the sample by a HLB solid-phase extraction column, and filtering the sample by a 0.22-micron filter membrane, performing analysis by pressurized capillary electrochromatography, performing detection at 270 nm with an ultraviolet detector by using a capillary electrochromatographic column with reversed-phase bonds and C18 as fillers as a detection column, wherein the mobile phase is acetonitrile and sodium dihydrogen phosphate (5 mmol/L, pH 6.0) with a ratio of 30:70 (V/V). The invention performs pretreatment of the sample by using a classic sample treatment method of liquid-liquid extraction combined with solid-phase extraction, and effectively reduces the content of impurities in fish flesh tissue and matrix interference; the capillary electrochromatography is adopted for analysis and detection, which has less organic reagent consumption; with the application of an external voltage, the retention time of 5 sulfonamides is reduced; the sensitivity is improved; 5 sulfonamides are separated and detected simultaneously; the method of the invention not only meets routine detection of eel sulfonamide residual quantities, but also is applicable to the detection of sulfonamides in other aquatic product samples.
Description
technical field [0001] The invention belongs to the field of food safety-veterinary drug residue detection, and relates to an analysis method for detecting sulfa drugs in eels by using capillary electrochromatography, specifically, using capillary electrochromatography to simultaneously measure sulfadiazine and sulfamethoxine in fish meat , sulfaquinoxaline, sulfamethoxazole, sulfamethoxazole five kinds of sulfa drugs. Background technique [0002] Sulfonamide drugs refer to the general term of a class of drugs with p-aminobenzenesulfonamide structure, which is a class of chemotherapeutic drugs for the prevention and treatment of bacterial infectious diseases. Because of its wide antibacterial spectrum, anti-coccidial and cheap and easy to obtain, it is still widely used in veterinary clinics and animal husbandry. Sulfa drugs are a class of antibacterial drugs that are allowed to be used in a limited amount by the state and can be used by feed producers. At present, the na...
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Login to view more IPC IPC(8): G01N30/02G01N30/06G01N30/74
Inventor 王阳光欧阳小琨董洁莹杨立业李大东
Owner ZHEJIANG OCEAN UNIV
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