An analytical method for the determination of multiple veterinary drug residues in aquaculture water
An analysis method, a technology for veterinary drug residues, applied in the field of food chemical analysis, can solve the problems of lack of qualitative accuracy, environmental pollution, low sensitivity, etc., and achieve the effects of reducing toxicity, saving analysis time, and good reproducibility
Active Publication Date: 2020-03-27
INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE
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Problems solved by technology
Among them, ELISA is prone to false positive results and cross-reactions; HPLC has poor anti-interference ability, low sensitivity and cannot meet the requirements of standard limits; GC-MS method requires tedious derivatization of samples; LC-MS / MS technology does not require derivatization treatment, and still has good selectivity, sensitivity and specificity under the condition of simultaneous detection of multiple components, making up for the shortcomings of the previous methods, but it is difficult to fully elucidate compounds The structural cleavage information is still lacking in qualitative accuracy, and it is easy to produce false positive results
The pretreatment methods for the detection of veterinary drug residues in aquaculture water include solid-phase extraction, liquid-liquid extraction and other methods. These methods use a lot of organic reagents, which are easy to pollute the environment, and the experiment takes a long time.
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[0041] (1) Standard solution preparation: Accurately weigh about 5.0 mg of cloxacillin sodium and disodium penicillin sodium salt hydrate standard substance, put them in respective 5mL volumetric flasks, and use acetonitrile aqueous solution (acetonitrile:water=30:70, v / v) Dissolve and adjust the volume to the mark to prepare a standard stock solution with a mass concentration of 1 mg / mL; accurately weigh 2-amino-5-benzimidazole, toltrazuril, clarazuril, salicylic acid, Acid, 4-aminoantipyrine, 4-formylaminoantipyrine, 4-methylaminoantipyrine, phenylbutazone, 17α-hydroxyprogesterone, melengestrol acetate, medigestrol acetate Ketone, medroxyprogesterone, carprofen, diclazuril, diclofenac, mefenamic acid, nabumetone and toltrazuril sulfone standard about 5.0mg, in the respective 5mL volumetric flask, dissolved with acetonitrile and Dilute to the mark, make a standard stock solution with a mass concentration of 1mg / mL, and store it in a refrigerator at 4°C;
[0042] (2) Ultraso...
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Abstract
The invention discloses an analytical method for determining multiple residues of veterinary drug in aquaculture water. The method comprises the following steps of: (1) preparing a standard solution; (2) performing ultrasound assisted extraction; (3) performing microextraction of a dispersing liquid; and (4) performing ultra-high performance liquid chromatography-high definition mass spectrometer analysis. The method disclosed by the invention can reduce use of a lot of organic solvents which are harmful to human body, has the advantages of being sensitive, accurate, time-saving, stable, high in precision, good in repeatability and the like, and is suitable for detecting aquaculture water samples in large batch.
Description
【Technical field】 [0001] The invention relates to an analysis method for determining residues of veterinary drugs in aquaculture water, in particular to an analysis method for determining residues of veterinary drugs in aquaculture water using ultrasonic-assisted dispersion liquid-liquid microextraction-ultra-high performance liquid chromatography-high resolution mass spectrometry, which belongs to food chemistry Analyze technical fields. 【Background technique】 [0002] The modern aquaculture industry tends to be large-scale and intensive, and the use of antibiotics and hormones has become an indispensable part of the development of the aquatic product aquaculture industry. However, due to the lack of scientific knowledge and the drive of economic interests, the phenomenon of drug abuse in the aquatic product farming industry is widespread, especially in our country. The direct consequence of the abuse of veterinary drugs is the residue of veterinary drugs in animal food, w...
Claims
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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 张宪臣华洪波李浩洋张朋杰卢俊文容裕棠
Owner INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE