| Virginiamycin(VGM)has been widely used as a growth promoting feed additive for livestock and poultry,which can also be used to treat diseases such as a liver abscess in cattle and necrotizing enteritis in chickens.Studies have found that the continuous use of VGM may increase the possibility of streptomycin resistant of Enterococcus faecium in humans.To avoid the existence of cross-resistance,VGM is gradually banned to promote the growth of livestock and poultry as a feed additive.GB/T 20765-2006 uses liquid chromatography-tandem mass spectrometry for the detection of VGM-M1 in muscle,liver,and kidney tissues of pigs.However,the scope of application of VGM is for pigs and poultry.The test method specified in the national standard is difficult to meet the actual testing requirements.Therefore,more comprehensive and faster detection methods are needed,but previous studies have always focused on the edible tissues of pigs and chickens,feed,egg and milk,even soil and has rarely addressed duck and goose tissues.Thus,it is necessary to supplement the detection of VGMM1 in edible tissues of ducks and geese.In this study,an ultra-performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS)method was developed for the determination of VGM-M1 in muscle,liver,kidney,and sebum tissues of ducks and geese.The tissue samples were extracted with acetonitrile,and the extracted supernatant was degreased with n-hexane,and fixed to volume with ultrapure water,after filtration and quantified by external standard method,and were determined by UPLC-MS/MS.Separated on a Waters Atlantis UPLC BEH C18 liquid chromatography column(1.7 μm,2.1 × 100 mm)and by using a multistage reaction monitoring method in positive ion detection mode with 0.1%formic acid wateracetonitrile as mobile phase.In the positive ion mode,the multi-stage reaction monitoring mode is selected,and two pairs of ion pairs 526.3>355.1 and 526.3>337.1 are selected as qualitative and quantitative ions for mass spectrometry detection.Through experiments,VGM-M1 has good resolution,uniform and symmetrical peak shape and appropriate retention time in this method.The conditions of liquid chromatography and mass spectrometry in this study can meet the detection of samples and can be used in subsequent tests.The established method was used to verify the edible tissues of ducks and geese,including muscle,liver,kidney and sebum.The detection limits of muscle,liver,kidney and sebum were 2.0 μg/kg,6.0μg/kg,8.0 μg/kg and 8.0μg/kg.The quantitative limits of muscle and other tissues were 10.0μg/kg and 50.0 μg/kg.VGM-M1 has a good linear relationship within the detection concentration range of 2～60ng/mL,and R2 is greater than 0.99.The average recovery of edible tissues of ducks was more than 88.7%,and the RSD within and between batches was less than 15%.The average recoveries of edible tissues of geese were more than 83.40%,and the RSD within and between batches were less than 20%,indicating that the method has good repeatability and reproducibility.The detection method established in this study simplifies the sample processing process,shortens the detection process,and optimizes the conditions of liquid chromatography and mass spectrometry.After a series of methodological verification,this method can specifically detect VGM-M1,has good sensitivity,presents a good linear relationship in the quantitative range,and has good repeatability and reproducibility.All indicators meet the requirements of veterinary drug residue specifications,and can be used for the detection of actual samples,it can also be used for market monitoring,laying the test foundation for the formulation of standard detection methods and providing feasible methods. |
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