高效液相色谱-串联质谱法同时测定畜禽组织和牛奶中螺旋霉素Ⅰ及其代谢物残留量OA

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of spiramycin Ⅰ and its metabolite(neospiramycin Ⅰ)in livestock and poultry tissues and milk.After extraction of the samples with hydroxymethyl amino-methane(Tris)and precipitation of proteins with metaphosphoric acid,the extracts were purified with HLB columns.The extracts were separated on a reversed-phase C18 column(100 mm×2.1 mm,2.7 μm)by gradient elution with acetonitrile and 0.1％formic acid aqueous solution.Tandem mass spectrometry with electrospray ionization was used to carry out quantitative analysis in positive ion and multiple reaction monitoring(MRM)mode by external standard method.The extraction solution,the types of SPE columns,and pH of the working solutions were evaluated.The chromatographic con-ditions and mass spectrometric parameters were optimized.The results showed that excellent linearity was obtained in the range of 0.2-20.0 μg/L with the correlation coefficients(r)higher than 0.999.The limits of detection(LODs)were 10 μg/kg and the limits of quantification(LOQs)were 50 μg/kg for the target analytes.At spiked levels of 50-600 μg/kg,the average recoveries ranged from 71.8％to 102％,with relative standard deviations(RSDs)ranging from 1.7％to 8.5％.The method conforms to the criteria for quality control of veterinary drug residue analysis in foods and can be applied to the simultaneous detection of spiramycin Ⅰ and its metabolite in various matrices,including muscle,viscera,and milk from livestock and poultry.