Study on the method for determining chloramphenicol in fresh milk by high performance liquid chromatography mass spectrometry
To establish a method for the determination of chloramphenicol residues in fresh milk by UPLC MS/MS.The determination method in Determination of Chloramphenicol Residue in Milk by UPLC MS/MS(GB 29688-2013)was optimized.Take an appropriate amount of fresh milk,add chloramphenicol-D5 internal standard,extract it with acetonitrile,centrifugate it at 5 000 r/min,pass it through OASIS Prime HLB col-umn,blow the solution dry with nitrogen,redissolve it in water,take the lower layer of aqueous solution and pass it through 0.22 μm aqueous filter membrane.Take C18 column as the liquid chromatographic column,elute according to the volume ratio of acetonitrile:water(60:40).The accuracy of chloramphenicol was better in the range of 0.2-10.0 μg/kg,and the correlation coefficients were greater than 0.99.The detection limit was 0.05 μg/kg,and the quantification limit was 0.2 μg/kg.The average recovery of chloramphenicol at three spiked concentrations(0.2,1.0,10.0 μg/kg)was 85.5％-116.0％,and the relative standard deviation was 1.23％-8.16％.The test results fully meet the requirements of relevant national standards for the detection of fresh milk,and are suitable for the qualitative and quantitative detection of chloramphenicol in fresh milk.
NETL
NSTL
万方数据
维普
