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Method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry

A technology of time-of-flight mass spectrometry and ultra-high performance liquid phase, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of affecting the natural environment such as soil, water and air, the decline of product output, and the decline of body immunity, so as to improve The degree of ionization and detection sensitivity, good stability, and the effect of improving accuracy

Inactive Publication Date: 2019-06-21
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, some unscrupulous merchants have not followed the NY 5071-2002 "Usage Guidelines for Pollution-Free Food and Fishery Drugs" issued by the Ministry of Agriculture in the process of increasing fisheries, neglected the ecological environment of water areas, and put in feed and used fishery drugs. , there are problems such as abuse, blindly increasing the dosage or the time of medication, which will lead to the deterioration of water quality, leading to various diseases, and then illegal medication again, forming a vicious circle
[0003] At present, the common drug residues mainly include antibiotics such as quinolones, tetracyclines, macrolides, sulfonamides, and chloramphenicol, and pigment drugs such as Sudan red and rhodamine. These drugs will eventually be passed on to humans and animals through the food chain , thereby affecting human health, leading to a decline in body immunity, damage to the nervous system, endocrine and reproductive systems, etc.; at the same time affecting the production and import and export of aquatic products, resulting in a substantial decline in product production; it will also affect the natural environment such as soil, water and air, Therefore, it is necessary to screen common drug residues in fish. However, most of the prior art is single-drug screening, lacking the simultaneous screening of enrofloxacin, dafloxacin, tetracycline, oxytetracycline, aureomycin, Doxycycline, chloramphenicol, thiamphenicol, florfenicol, sulfamethiadiazole, sulfamethoxypyridazine, sulfathiazole, sulfadiazine, sulfadoxine, sulfisoxazole, sulfabenzopyrazole, Sulfacetamide, sulfamethazine, azithromycin, tilmicosin, midecamycin, roxithromycin, acetylspiramycin, doramectin, Sudan red Ⅰ, Sudan red Ⅱ, Sudan red Ⅲ, Sudan red Method for 29 drugs in 6 categories including IV and Rhodamine B

Method used

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  • Method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry
  • Method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry
  • Method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0103] Weigh 2.0g of homogenized cod muscle sample A into a 50mL centrifuge tube, add 2.0mL of methanol, and adjust the volume to 12.5mL with acetonitrile aqueous solution acidified with acetic acid, wherein the acetonitrile aqueous solution contains 0.1% acetic acid and 16% water, and then add 2.5 mL0.1mol / L and pH=4.0±0.1 Na 2 EDTA-Mcllvaine buffer solution, shake and vortex; add anhydrous magnesium sulfate 3.0g, sodium acetate 1.9g and sodium chloride 1.5g, shake and vortex, centrifuge at 6000r / min for 8min; take the supernatant into a test tube, add C18 0.4g, PSA 0.4g and 0.1g anhydrous magnesium sulfate, vortex, centrifuge at 6000r / min for 8min, take the supernatant, filter through a 0.22μm filter membrane to obtain blank matrix sample solution A. The full-scan analysis of the target drugs was carried out in the first-order mass spectrometry acquisition mode, and the qualitative analysis of 29 target drugs was carried out by comparing the retention time with the standard ...

Embodiment 2

[0105] Weigh 5.0g of homogenized cod muscle sample B into a 50mL centrifuge tube, add 3.0mL of methanol, and adjust the volume to 12.5mL with an aqueous solution of acetonitrile acidified with acetic acid, wherein the aqueous solution of acetonitrile contains 0.1% acetic acid and 16% of water, and then add 2.5 mL0.1mol / L and pH=4.0±0.1 Na 2 EDTA-Mcllvaine buffer solution, shake and vortex; add 6.0g of anhydrous magnesium sulfate, 1.9g of sodium acetate and 1.5g of sodium chloride, shake and vortex, centrifuge at 8000r / min for 10min; take the supernatant into a test tube, add C18 0.4g, PSA 0.4g and 0.5g anhydrous magnesium sulfate, vortex, centrifuge at 8000r / min for 10min, take the supernatant, filter it through a 0.22μm filter membrane to obtain the blank matrix sample solution B. The full-scan analysis of the target drugs was carried out in the first-order mass spectrometry acquisition mode, and the qualitative analysis of 29 target drugs was carried out by comparing the ret...

Embodiment 3

[0107] Weigh 3.0g of homogenized cod muscle sample C into a 50mL centrifuge tube, add 2.5mL of methanol, use acetic acid acidified acetonitrile aqueous solution to make up to 12.5mL, wherein the acetonitrile aqueous solution contains 0.1% acetic acid and 16% water, then add 2.5 mL0.1mol / L and pH=4.0±0.1 Na 2 EDTA-Mcllvaine buffer solution, shake and vortex; add 6.0g of anhydrous magnesium sulfate, 1.9g of sodium acetate and 1.5g of sodium chloride, shake and vortex, centrifuge at 8000r / min for 6min; take the supernatant into a test tube, add C18 0.4g, PSA 0.4g and 0.3g anhydrous magnesium sulfate, vortex, centrifuge at 7000r / min for 6min, take the supernatant, and filter through a 0.22μm filter membrane to obtain the blank matrix sample solution C. The full-scan analysis of the target drugs was carried out in the first-order mass spectrometry acquisition mode, and the qualitative analysis of 29 target drugs was carried out by comparing the retention time with the standard subs...

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Abstract

The invention relates to a method for simultaneously screening multiples categories of drug residues in fish by using ultra performance liquid chromatography-quadrupole rod time-of-flight mass spectrometry. The multiples categories of drugs screened simultaneously comprise enrofloxacin, danofloxacin, tetracycline, oxytetracycline , chlortetracycline, doxycycline, chloramphenicol, thiamphenicol, florfenicol, sulfamethoxazole, sulfamethoxazole, sulfathiazole, sulfadiazine, sulfadoxine, sulfisoxazole, sulfaphenirazole, sulfacetamide, sulfamethazine, azithromycin, tilmicosin, medimycin, roxithromycin, acetylspiramycin, doramectin, sudan I, sudan II, sudan III, sudan IV and rhodamine B. By optimizing the parameters of a d-SPE pretreatment method, all target drugs can obtain good recovery rates.29 kinds of target drugs are simultaneously screened by an optimized chromatographic mass spectrometry condition, thereby achieving simultaneous screening of common multiples categories of drug residues in fish. The method has a good application prospect in the field of fish food.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and specifically relates to a method for simultaneously screening multi-category drug residues in fish by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Background technique [0002] Fish and fish products are one of the main dietary sources, and they are also the types with a high incidence of food safety incidents. In the past two years, problems have occurred frequently. The "China Food Safety Development Report 2016" pointed out that 13 kinds of aquatic products such as shrimp and fish have safety problems. The pass rate has been lower than 96% for three consecutive years, and the safety factor needs to be improved. The primary problem in the quality and safety of fish food is excessive drug residues. In recent years, some unscrupulous merchants have not followed the NY 5071-2002 "Usage Guidelines for Pollution-Free Food and Fishery Dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 贾玮张焱茜
Owner SHAANXI UNIV OF SCI & TECH
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