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、四环素类和大环内脂类抗生素.docx

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、四环素类和大环内脂类抗生素王硕1 张晶2 邵兵2*（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）摘要：本文采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了城市污水处理厂污泥中50种抗生素（氯霉素、磺胺、喹诺酮、四环素和大环内脂类）的分析方法。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；ACQUITYUPLCBEH C18 柱用作色谱分离，流动相为0.1%甲酸水溶液-甲醇（ESI+）和乙腈-水（ESI-），梯 度洗脱；质谱采集使用多反应监测(MRM)模式；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0.50～400 μg/L，相关系数均大于0.99。方法定量限为0.1～5.0 μg/kg，三个加标水平的回收率为40.1%～111.1%，相对标准偏差为2.9%～27.1%，满足环境样品中痕 量污染物检测的需要。应用此方法对北京某污水处理厂活性污泥和剩余污泥开展调查，共检出14种药物，包括磺胺嘧啶、磺胺吡啶、磺胺甲恶唑、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。关键词：磺胺；喹诺酮；四环素；大环内脂；氯霉素；液相色谱-串联质谱；污泥Analysis of chloramphenicol, sulfonamides,fluoroquinolones,tetracyclines and macrolides in sewage sludge by ultraperformanceliquid chromatography tandem massspectrometryWang Shuo1 Zhang Jing2 ShaoBing2*(1. Chaoyang District Center for Disease Control and Prevention, Beijing 100021; 2. Beijing Key Laboratoryof DiagnosticandTraceabilityTechnologiesforFoodPoisoning,BeijingCenterforDiseaseControlandPrevention, Beijing100013)1Abstract:Acomprehensivemethodwasdevelopedforsimultaneousanalysisof50antibioticdrugs,includingchloramphenirol, sulfonamides, fluoroquinolones, tetracyclines and macrolides in sewage sludge byultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sludge sampleswereultrasonicallyextractedbyacetonitrile-watersolutionandthencentrifugated.ThesupernatantwereconcentratedbyanOasisHLBsolid-phaseextraction(SPE)cartridgeandpurifiedbyanaminoSPEcartridge.Theseparationof50targetdrugswasconductedonanACQUITY UPLCBEHC18columnusingamobilephaseof0.1%formicacid – methanol (ESI+) or acetonitrile – water (ESI-) with gradient elution. A multiple reaction monitoring(MRM)wasemployedinmassspectrometryacquisition.Thematrix-matchedexternalstandardscalibrationwasusedforquantitation.Goodlinearityoftheanalyteswasachievedover0.50～400μg/L,withthecorrelationcoefficients基金项目：国家自然科学基金*通讯作者，