HPLC-MS/MS法测定水产品中硫酸粘素、杆菌肽及维吉尼霉素M1的残留量

A high performance liquid chromatography tandem mass spectrometric(HPLC-MS/MS) method was established to simultaneously detect colistin sulfuric(CS),bacitracin(BTC) and virginiamycin M1(VGMM1) in aquatic products.We extracted the samples with methanol-0.1% formicacid(V:V=2:5),removed their protein with 4% TCA acetonitril,removed fat with acetonitrile saturated n-hexane,and then cleaned them up with OASiS HLB solid phase extraction(SPE) column.Next,we detected the analytes by HPLC-MS/MS under the selected reaction monitoring mode and quantified them by external standard method.Results show that CS and BTC have good linearity between the peak areas in concentrations ranged 0.01~10.00 mg · L-1,VGMM1 as well in concentrations ranged 0.002~2.000 mg · L-1,and the correlation coefficients(R2) are all more than 0.995.The detection limits of CS,BTC and VGMM1 are 10 μg · kg-1,10 μg · kg-1and 2 μg · kg-1 respectively,and the quantification limits are 20 μg · kg-1,20 μg · kg-1 and 4 μg · kg-1respectively.Three samples in three different concentration levels are chosen for recovery,getting a 72.3%~103.9% average recovery rate,and a relative standard deviations varying from 1.10%~10.92%.In conclusion,method proposed has advantages of simplicity,sensitivity and repeatability,which provide technical support for the detection of these 3 kinds of drug residues in aquatic products.