Liquid chromatography-mass spectrometry method for detecting 45 veterinary drugs in pond sediment

A liquid mass spectrometry and sediment technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of lack of national standard methods and effective technical guidance, and achieve the effects of high sensitivity, small matrix interference, and strong purification effect

Inactive Publication Date: 2018-01-09
SOUTH CHINA SEA FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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For the simultaneous monitoring of multiple drug residues in pond sediments, there i

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  • Liquid chromatography-mass spectrometry method for detecting 45 veterinary drugs in pond sediment
  • Liquid chromatography-mass spectrometry method for detecting 45 veterinary drugs in pond sediment
  • Liquid chromatography-mass spectrometry method for detecting 45 veterinary drugs in pond sediment

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[0021] The technical solutions of the present invention will be further described below with reference to specific embodiments, which are only used to explain the present invention, and are not intended to limit the present invention.

[0022] The technical scheme adopted in the present invention is:

[0023] 1) Extraction of samples: Take an appropriate amount of sediment sample, spread a layer evenly on the filter paper, place it in a cool and dry place, dry it in the dark, then collect the sample and crush it, accurately weigh 2.00g of the sample into a 50mL plastic centrifuge tube, add 0.4gNa 2 .EDTA, and 20 mL of mixed extraction reagent, vortex for 2 min, ultrasonic extraction for 20 min, centrifuge at 4000 r / min for 10 min, accurately measure 10 mL of supernatant, add distilled water to dilute to 50 mL, adjust pH to 2.8-3.0 with formic acid, and then purify;

[0024] 2) Solid phase extraction purification: 500mg / 6mL HLB solid phase extraction cartridge was sequentially...

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Abstract

The invention provides a liquid chromatography-mass spectrometry method for detecting 45 veterinary drugs in pond sediment. The liquid chromatography-mass spectrometry method comprises the following steps: 1) extracting a sample; 2) purifying through solid phase extraction; 3) analyzing through liquid chromatography-mass spectrometry: measuring a filtrate in the step 2) by using a liquid chromatograph-tandem mass spectrometer to obtain the peak area of a substance to be measured, substituting the peak area into a corresponding standard curve, and analyzing and calculating to quantitatively obtain the contents of the 45 veterinary drugs in the sediment sample. The high-performance liquid chromatograph-tandem mass spectrometer is used, the liquid chromatography-mass spectrometry method is based on the difference between the polarities of various compounds, the chromatographic column uses a Kinetex C18 chromatographic column having relatively high column efficiency and having the particlesize of 1.7 microns, positive and negative ions are simultaneously scanned, simultaneous analysis of the 45 veterinary drugs can be achieved during an experiment, and high-throughput and high-sensitivity rapid detection requirements can be met.

Description

technical field [0001] The invention relates to a method for detecting 45 kinds of veterinary drugs, in particular to a method for detecting 45 kinds of veterinary drugs in pond sediments by liquid mass spectrometry. technical background [0002] In the process of aquaculture, in order to prevent or treat bacterial diseases of fish, shrimp and other animals and reduce economic losses, relevant practitioners often use antibacterial drugs such as sulfonamides, fluoroquinolones, tetracyclines, macrolides, and even nitric acid. Prohibited drugs such as furans and chloramphenicol are also frequently detected in aquatic products. Different from livestock and poultry farming, no matter in aquaculture, whether the drug is mixed in the feed or directly poured into the pond, the drug will dissolve in the water body, then accumulate in the sediment, and slowly release into the water body as the external environment changes. release, resulting in secondary pollution, and the residual d...

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IPC IPC(8): G01N30/88G01N30/06
Inventor 赵东豪王强王旭峰黎智广黄珂杨宏亮蔡楠关婉琪李刘冬柯常亮刘奇陈洁文莫梦松
Owner SOUTH CHINA SEA FISHERIES RES INST CHINESE ACAD OF FISHERY SCI
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