The Application Of QuEChERS Pretreatment Technology In The Detection Of Four Kinds Of Veterinary Drugs Residues In Marine Products

Residues of veterinary drugs in marine products have been banned,but no effective.Sulfonamides,Quinolones,Tetracyclines,and other veterinary drugs such as malachite green are used more often than not,and they have brought serious potential harm to human health and life safety through the transmission of the food chain.Oyster,scallop,squid,and cuttlefish are soft-shelled marine products that people consume more.They can easily cause residues of various veterinary drugs and banned compounds during growth and reproduction.Therefore,it is very important to establish an efficient,sensitive and simple method for multi-residue detection of veterinary drugs in marine products that can be used for qualitative and quantitative analysis of the analytes.In this paper,the QuEChERS sample preparation method combined with the high-performance liquid chromatography tandem triple quadrupole mass spectrometry detection method was used to establish the rapid,high-efficiency,and high-sensitivity multi-residue detection method for 21 kinds of veterinary drugs and banned compounds of Sulfanilamides(Sulfamethazine,Sulfamonomethoxine,Sulfamethoxazole,Sulfadimethoxine),Quinolones(Norfloxacin,Ofloxacin,Pefloxacin,Lomefloxacin,Danofloxacin,Enrofloxacin,Sarafloxacin,Difloxacin,Oxilinic acid,Flumequine,Ciprofloxacin),Tetracyclines(Oxytetracycline,Tetracycline,Chlortetracycline,and Doxycycline),Malachite green and Leucomalachite green in oyster,scallop,squid,and cuttlefish.A sample of 2.00 g was added to acetonitrile containing 1%acetic acid,anhydrous sodium sulfate,sodium chloride,vortex mixed,ultrasonic extraction,centrifugation,repeated extraction,and two extractions were combined to add 400 mg PSA,400 mg C18,1200 Magnesium sulfate in polypropylene centrifuge tubes,vortexed,and centrifuged.The supernatant was passed through a 0.22 μm organic microfiltration membrane.HPLC conditions,column temperature:40℃;flow rate:0.3 mL/min;injection volume:5μL;column:ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7 ×m);mobile phase A:containing 0.1%formic acid-Aqueous solution,mobile phase B:pure acetonitrile,gradient elution.The electrospray ionization source(ESI source),positive ion scan mode,multiple reaction monitoring mode(MRM)were used for scanning,external standard method for quantification.The 21 compounds had good linearity in the corresponding range,and the correlation coefficient r was greater than 0.9995.The total recoveries of the four classes of 21 compounds in the four soft shellfish products of oyster,scallop,squid and cuttlefish were within the range of 65.26%～113.5%.The relative standard deviation was less than 6.78%and the method had good repeatability.The intra-day and inter-day precision of 21 compounds tested were less than 6.26%and 6.02%,respectively,which met the testing requirements.The detection limit of 21 compounds was 0.8 μg/kg and the limit of quantitation was 2.5 μg/kg.This method was applied to the residue of four types of 21 compounds in four kinds of soft shellfish products including 150 oyster,scallop,squid and cuttlefish in 8 regions including Shenzhen,Dongguan,Zhaoqing,Shantou,Maoming,Jiangmen,Shanwei and Huizhou in Guangdong Province.conduct the test.The results showed that none of the 150 samples were detected.In summary,the detection method has good reproducibility,high sensitivity,and reliable results.It is four kinds of oyster,scallop,squid,and cuttlefish in four kinds of soft marine products:sulfonamides,quinolones,tetracyclines,and malachite green.The residue detection of 21 compounds provides a technical support.