【摘要】 目的建立超高效液相色谱-串联质谱法同时检测水源水和自来水中的磺胺类、β-内酰胺类、四环素类、氯霉素类40种抗生素,同时建立超高效液相色谱-三重四级杆飞行时间质谱的确认方法。方法水样经离心沉淀除去颗粒物,盐酸调至p H=3,经HLB固相萃取小柱富集、净化,甲醇洗脱,洗脱液浓缩后进超高效液相色谱-串联质谱分析。高含量样品通过进一步浓缩,采用三重四级杆飞行时间质谱进行确认。结果 40种抗生素在0.5 ng/ml~20 ng/ml时,线性关系较好,相关系数(r)≥0.997,检出限为1 ng/L~5 ng/L,定量限为3 ng/L~10 ng/L。在低(10 ng/L)、中(50 ng/L)、高(100 ng/L)3种加标浓度下,40种抗生素的回收率为40.28%~120.50%,相对标准偏差(RSD)为1.25%~13.22%。同时,高含量样品经三重四级杆飞行时间质谱得到进一步验证,确保了结果的准确性。结论该方法简单、快速、准确,适用于水源水和自来水中抗生素的多残留检测。更多还原

【Abstract】 Objective To develop a method for simultaneous determination of 40 kinds of antibiotics including sulfonamides,β-Lactams,tetracyclines,chloramphenicols in source water and tap water by ultra-performance liquid chromatography tandem mass spectrum( UPLC-MS / MS). Methods Particulate matter was dislodged from water sample by centrifugation,adjusting the p H to 3 by hydrochloric acid,and oasis HLB solid phase extraction column( SPE) was used for the concentration and purification,methanol elute,and the elution was concentrated before UPLC-MS / MS analysis. Results Good linearity was obtained when the concentration of the 40 antibiotics were within 0. 5 ng / ml-20. 0 ng / ml,with correlation coefficient( r) ≥0. 997 and the limits of determination( LOD) within 1 ng / L-5 ng / L and the limits of quantification( LOQ) within 3 ng / L-10 ng / L,respectively. The recovery were from 40. 28% to 120. 50%,and the RSD of inner-day precision of them were within1. 25%-13. 22% in 3 spike levels( 10 ng / L,50 ng / L,100 ng / L) of 40 kinds antibiotics. Meanwhile,high concentration samples were confirmed by UPLC-Q-TOF so as to ensure the accuracy. Conclusion The established method is simple,rapid and accuracy,which can be applied to the determination and quantification of antibiotics residues in source water and trap water.更多还原