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

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...

Examples

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...

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...

Examples

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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