超高效液相色谱-串联质谱筛查确证尿液中磺胺、喹诺酮与四环素抗生素

Study on the Method for the Identification of Sulfanilamide,Quino⁃lone and Tetracycline in Urine by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定尿液中磺胺类、四环素类、喹诺酮类共45种抗生素的检测方法。尿液样品经提取后,采用HLB固相萃取柱(200 mg/6 mL)净化,使用ThermoAccu-core RP-MS(100 mm×2.1 mm,2.6µm)色谱柱进行分离,以乙腈-0.02%甲酸溶液为流动相梯度洗脱。在正离子扫描模式下(ESI+),以选择反应监测模式(SRM)检测,外标法定量。45种目标化合物在3个加标水平(2.0、5.0、10.0µg/L)下的回收率为78.6%~114%,相对标准偏差为0.60%~18%;方法的检出限为0.1~0.5µg/L,定量下限为0.3~1µg/L。将所建方法用于280个尿液样品中抗生素的检测,均未检测到抗生素残留。所建方法的精密度和准确度高,操作简单便捷,为尿液中抗生素残留的筛查提供了方法支持。

A confirmatory test for the simultaneous determination of sulfonamides,tetracyclines,and quinolones in urine totalling 45 antibiotics by ultra-high performance liquid chromatography-tan-dem mass spectrometry(UPLC-MS/MS)was developed.The urine samples were extracted and then cleaned up by an HLB solid phase extraction column(200 mg/6 mL),and the separation of the target was performed on a ThermoAccucore RP-MS column(100 mm×2.1 mm,2.6µm)using acetoni-trile-0.02%formic acid aqueous solution with gradient separation elution,detected in positive ion scanning mode(ESI+)in multiple selected reaction monitoring(SRM)and quantified by external stan-dard method.The recoveries of a total of 45 target compounds from three classes of antibiotics at three spiked levels(2.0,5.0 and 10.0µg/L)were in the range of 78.6%-114%with the RSDs in the range of 0.60%-18%,and the limits of detection(LODs)and the limits of quantification(LOQs)of the method were in the range of 0.1-0.5µg/L and 0.3-1µg/L,respectively.The developed meth-od was applied to 280 urine samples for the detection of antibiotics,none of which detected antibiot-ics residues in excess of limit.The results showed that the established method was highly precise and accurate,simple and convenient,and included commonly used antibiotic species,which can support the screening antibiotic residues in urine.