Determination of Four Tetracyclines Residues in Milk Powder by Liquid Chromatography-Tandem Mass Spectrometry
A method for simultaneous determination of tetracycline,oxytetracycline,chlortetracycline and doxycycline residues in milk powder by liquid chromatography-tandem mass spectrometry was established.Milk powder samples were extracted with 0.1 mol/L Mcllvaine-Na2EDTA buffer solution,purified by HLB solid phase extraction column,eluted with 0.1％ formic acid solution and methanol as mobile phase gradient elution,separated by C18 column,electrospray positive ion mode scanning,multiple reaction monitoring(MRM),matrix adding standard curve and internal standard method for quantification.The results showed that the linearity of the four tetracyclines were good,and the correlation coefficients(R2)were all more than 0.995.In powdered milk,the detection limits for tetracycline,oxytetracycline,and chlortetracycline are 0.4 μg/kg,with quantification limits of 1 μg/kg as for doxycycline,the detection and quantification limits are 1 μg/kg and 3 μg/kg.The recoveries of the four compounds are between 91.8％ and 104.0％ at low,medium and high concentration levels,and the relative standard deviations are between 2.1％ and 4.3％.Verified by methodology and applied to the detection of tetracycline quality control samples in milk powder,it is proved that this method has high sensitivity,good reproducibility and accurate results,and can provide technical reference for daily detection of tetracycline antibiotics in milk powder.
liquid chromatography-tandem mass spectrometrytetracyclinesmilk powderresidue
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