超高效液相色谱-串联质谱法同时测定牛肉中3类31种药物残留检测方法的建立

Determination of Thirty-one Veterinary Residues in Beef by UPLC-MS/MS

采用超高效液相色谱-串联质谱方法(UPLC-MS/MS)同时测定牛肉中3种四环素类药物、11种喹诺酮类药物和17种磺胺类药物的残留。采用Mcllvaine-Na_2EDTA缓冲液和磷酸盐缓冲液作为提取液,经HLB固相萃取柱净化,氮气吹干,复溶后,供UPLC-MS/MS测定。液相色谱条件为:色谱柱为Waters BEH C18柱(50 mm×2.1 mm,1.7μm);流动相为乙腈-0.1%甲酸水溶液,梯度洗脱;柱温为40℃;流速为0.3 mL/min;进样量:2μL。质谱条件为:电喷雾离子源(ESI^+),多反应监测(MRM)方式采集,外标法定量。结果表明:在5~500μg/L的系列浓度范围内,31种药物药物的相关系数r>0.990;方法检测限为5μg/kg,定量限为10μg/kg;从10、50、100μg/L 3个添加浓度检测结果可以看出,方法的平均回收率在60%~110%,批内、批间RSD均小于20%。该方法可作为牛肉中这3类药物残留的确证方法。

Residues in 3 tetracyclines, 11 quinolones and 17 sulfonamides in beef were determined by UPLC-MS/MS. The samples were extracted by Mcllvaine-Na_2EDTA and phosphate buffer solution, purified by HLB solid phase extraction column, blow-dried by nitrogen and determined by UPLC-MS/MS after being redissolved. Waters BEH C18 column（50 mm×2.1 mm, 1.7 μm） was chosen to be chromatographic column; acetonitrile was chosen to be mobile phase and the samples were eluted gradiently; temperature of the column was 40 ℃; flow velocity was 0.3 mL/min; sample size was 2 μL. Electrospray ionization source（ESI＋）, acquisition by multiple reaction monitoring and quantification by external standard method were included in mass spectrometry. The result showed that the good linearity was obtained within the mass concentration range of 5 -500 μg/L（r20.990）; the LOD was 5 μg/kg and LOQ was 10 μg/kg. The average recovery was 60%-110%, when 10, 50 and 100 μg/L drugs were added into the beef, and the RSD was less than 20%. The method is accurate, which is satisfied to determination of the thirty-one veterinary residues in beef.