超高效液相色谱-串联质谱测定污泥中氯霉素、磺胺类、喹诺酮类、四环素类与大环内酯类抗生素  

Analysis of Chloramphenicol,Sulfonamides,Fluoroquinolones,Tetracyclines and Macrolides in Sewage Sludge by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王硕[1] 张晶[2] 邵兵[2] 

机构地区：[1]北京市朝阳区疾病预防控制中心,北京100021 [2]北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京100013

出　　处：《分析测试学报》2013年第2期179-185,共7页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20837003)

摘　　要：建立了测定城市污水处理厂污泥中50种抗生素(氯霉素、磺胺、喹诺酮、四环素和大环内酯类)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。污泥样品经乙腈-水溶液超声萃取,高速冷冻离心后,提取液经过HLB柱富集和NH2柱净化;ACQUITY UPLC BEH C18柱用作色谱分离,以0.1%甲酸水溶液-甲醇(ESI+)和乙腈-水(ESI-)为流动相进行梯度洗脱;多反应监测(MRM)模式进行检测;目标药物使用基质外标法定量。50种目标药物的线性范围为0.50～400μg/L,相关系数均大于0.99。方法定量下限为0.10～5.00μg/kg,3个加标水平下的回收率为40%～111%,相对标准偏差为2.9%～27.1%。应用此方法对北京某污水处理厂活性污泥和剩余污泥进行检测,共检出14种药物,包括磺胺嘧啶、磺胺吡啶、磺胺甲唑、吡哌酸、氧氟沙星、依诺沙星、培氟沙星、诺氟沙星、环丙沙星、恩诺沙星、洛美沙星、斯帕沙星、土霉素和阿奇霉素,其浓度为1.2～442.5μg/kg。该方法简便快速、灵敏可靠,适用于污泥中多种抗生素药物残留的同时测定。A comprehensive method was developed for the simultaneous analysis of 50 antibiotic drugs, including chloramphenicol, sulfonamides, fluoroquinolones, tetracyclines and macrolides in sewage sludge by ultra performance liquid chromatography - tandem mass spectrometry （ UPLC - MS/ MS）. The sludge samples were ultrasonically extracted with acetonitrile -water solution and then centrifugated. The supernatant were concentrated with an Oasis HLB solid-phase extraction （SPE） cartridge and purified with an amino SPE cartridge. The separation of 50 target drugs was performed on an ACQUITY UPLC BEH Cls column using a mobile phase of O. 1% formic acid -methanol（ESI ＋ ） or acetonitrile - water （ ESI - ） by gradient elution. A multiple reaction monitoring （ MRM ） was employed in mass spectrometry acquisition. The matrix-matched external standard calibration was used for quantitation. Good linearities of the analytes were achieved over the concentration of 0. 50 - 400 μg/L, with correlation coefficients above 0. 99. The method quantitation limits（MQL） for target compounds were in the range of 0. 10 - 5.00 μg/kg. Average recoveries of 50 analytes at three spiked levels ranged from 40% to 111% with relative standard deviations（ RSDs ） of 2. 9% -27. 1%. The developed method was applied in the analysis samples from sewage treatment plants in Beijing, of target drugs in both activated and excess sludge while 14 target compounds, namely sulfadiazine,sulfapyridine, sulfamethoxazole, pipemdilic acid, ofloxacin, enoxacin, pefloxacin, norfloxacin, ciprofloxacin, enrofloxacin, lomefloxacin, sparfloxacin, oxytetracychne and azithromycin, were de- tected in the concentration range of 1.2 -442. 5 μg/kg. The method was rapid, sensitive and relia- ble, and was suitable for the simultaneous determination of 50 antibiotics in sludge sample.

关 键 词：磺胺 喹诺酮 四环素 大环内酯 氯霉素 液相色谱-串联质谱 污泥 

分 类 号：O657.63[理学—分析化学] S859.796[理学—化学]