超高效液相色谱-串联质谱法检测牛奶中10种四环素类药物残留

Detection of Ten Tetracycline Residues in Milk by UPLC-MS/MS

建立牛奶中10种四环素类兽药残留量的高效液相色谱-串联质谱法。样品经过EDTA-Mcllvaine缓冲液超声提取,经离心和过滤后,取10 mL上清液经固相萃取柱(Oasis PRiME HLB)净化。通过流动相(0.1%甲酸溶液-乙腈)梯度洗脱,经超高效液相色谱用ACQUITY UPLC BEH柱分离,进入质谱检测。结果表明,10种四环素类药物在2.5~80.0 ng·mL-1线性关系良好,R均达到0.995以上;检出限(S/N=3)均为0.5μg·kg^(-1);3个添加水平下的平均回收率在68.0%~101.2%,相对标准偏差为1.9%~11.6%(n=6),该方法可以满足四环素类兽药残留的定量分析。

A method for determination of tetracycline residues in milk by UPLC-MS/MS was developed.The target antibiotics in samples were extracted ultrasonically with EDTA-Mcllvaine solution.10 mL of the supernatant was purified by solid phase extraction column(Oasis PRiME HLB)after centrifugation and filtration.It was eluted by mobile phase(0.1%formic acid-acetonitrile)gradient,separated by ultra-high performance liquid chromatography with ACQUITY UPLC BEH column,and detected by mass spectrometry.The results indicate that between 2.5~80.0 ng·mL-1,ten tetracycline drugs have a good linear relationship,with R reaching above 0.995;The detection limit(S/N=3)is all 0.5μg·kg^(-1);The average recovery rate at three levels of addition ranges from 68.0%to 101.2%,with a relative standard deviation of 1.9%to 11.6%(n=6).This method can meet the quantitative analysis of tetracycline veterinary drug residues.