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A method for simultaneous detection of multiple antibiotic residues in vegetables
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A technology of antibiotics and vegetables, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high detection limit, high cost, and few types of antibiotics, and achieve the effect of overcoming high cost
Active Publication Date: 2019-02-19
INST OF AGRI RESOURCES & REGIONAL PLANNING CHINESE ACADEMY OF AGRI SCI
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[0004] The purpose of the present invention is to provide a method for detecting antibiotic residues in vegetable samples, that is, by effectively extracting antibiotics in vegetables, using high performance liquid chromatography tandem mass spectrometry under optimized liquid chromatography and mass spectrometry conditions to detect a variety of antibiotics in vegetable samples. Antibiotics are detected to overcome the shortcomings and deficiencies of the existing antibiotic detection methods, such as high cost, few types of antibiotics and high detection limit
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Embodiment 1
[0038] The determination of embodiment 1 standard curve, detection limit and quantitative limit
[0039] (1) Preparation of standard stock solution:
[0040] Accurately weigh 1mg of each of the 11 target antibiotic standards in a 10ml brown volumetric flask, dissolve and dilute to volume with the initial mobile phase (0.1% formic acid solution and acetonitrile, the ratio is 8:2), and prepare a 0.1mg / ml single standard stock solution, stored at 4°C.
[0041] Accurately pipette 10 μl of the 11 single-standard stock solutions into the same 10ml brown volumetric flask to make up the volume with the initial mobile phase, mix evenly after ultrasonication, and prepare a mixed standard solution with each antibiotic content of 100 μg / L ①.
[0042] Accurately pipette 5ml of the mixed standard solution into a 10ml brown volumetric flask with the initial mobile phase to make up the volume, mix evenly after ultrasonication, and prepare a mixed standard solution with each antibiotic conten...
Embodiment 2
[0058] Example 2 Verification, addition and recovery detection experiment
[0059] (1) Experimental steps
[0060] The collected antibiotic-free organic vegetable samples (leek, celery, lentils, beans, cauliflower), freeze-dried, ground through a 2mm sieve, accurately weighed 1g of the ground sample, mixed the antibiotic mixed standard solution in the vegetable sample to obtain 0.05 Fortified vegetable samples at μg / g, 0.1 μg / g and 0.5 μg / g. Then add 10ml of acetonitrile:hydrochloric acid (125:4, v / v) extractant, vortex for 30s, sonicate at room temperature for 15min, centrifuge at 8000rpm for 15min, and transfer the supernatant to another brown container. Then use the same method to extract the precipitate again, the steps are the same as above, combine the extracts and pass through a 0.45 μm membrane filter. Concentrate the combined extracts to 3-5 ml using a rotary evaporator.
[0061] Activation of the HLB column: first pass through the column naturally with 5ml of meth...
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Abstract
The invention relates to an antibiotic detection method. The method concretely comprises the following steps: (1) carrying out pretreatment for vegetable samples in order to obtain an antibiotic extract; (2) carrying out extraction for the antibiotic extract in order to obtain an antibiotic eluate; (3) evaporating the antibiotic eluate to dryness by a rotary evaporator, carrying out volumetric flask preparation with an initial mobile phase, and carrying out filtering with a syringe filter in order to obtain an antibiotic liquid to be measured; (4) carrying out detection for the antibiotic liquid to be measured by optimized high performance liquid chromatography-tandem mass spectrometry in order to detect antibiotics to be measured. The method for detecting 11 kinds of antibiotic residues in vegetable samples has the advantages of high recovery rate and low detection limit, and overcomes the disadvantages and insufficient that antibiotic detection methods in the prior art have high cost, few antibiotic detection kinds, and high detection limit; a base for assessing antibiotic environmental behaviors and risks is established.
Description
technical field [0001] The invention relates to an antibiotic detection method, in particular to a method for simultaneously detecting multiple antibiotic residues in vegetables by using high-performance liquid chromatography tandem mass spectrometry. Background technique [0002] Antibiotics refer to substances with the same or similar structure that are obtained from bacteria, actinomycetes, fungi and other microorganisms through cultivation or synthesized by chemical synthesis, and have the ability to kill or inhibit pathogenic microorganisms. In recent years, a large number of antibiotics have been widely used in livestock and poultry breeding as veterinary drugs and feed additives, and play an important role in the prevention and control of animal diseases, improving feed conversion efficiency, and promoting animal growth and development. However, antibiotics that enter animals through oral or intramuscular injection cannot be fully absorbed and utilized. The amount exc...
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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 李兆君张文娟刘元望冯瑶张彩月魏朝俊成登苗章程
Owner INST OF AGRI RESOURCES & REGIONAL PLANNING CHINESE ACADEMY OF AGRI SCI
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