目的 建立基于超高效液相色谱-四极杆-飞行时间质谱(ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry,UHPLC-Q-TOF-MS)技术快速筛查地表水中34种新兴污染物的方法.方法 通过正交试验设计优化固相萃取(solid phase extraction,SPE)前处理条件,样品经Oasis® HLB和Oasis® MCX固相萃取柱串联富集萃取.萃取物采用Kinetex® EVO C18色谱柱分离,0.1%甲酸水溶液和0.1%甲酸甲醇溶液梯度洗脱,Q-TOF-MS"fullscan"和"targeted MS/MS"模式检测34种新兴污染物,建立34种新兴污染物母离子、子离子及保留时间的数据库.结果 地表水中34种新兴污染物在各自线性范围内呈良好的线性关系,相关系数(r)大于0.97.检出限为0.2～10 ng/L,回收率为81.2%～119.2%,日间精密度为0.78%～18.70%.将方法应用于多份地表水样品的检测,共检出6种新兴污染物,质量浓度为1.93～157.71 ng/L.结论 该方法能简单、快速地对地表水中的多种痕量级新兴污染物进行筛查分析.
Abstract
Objective To establish a rapid screening method for 34 emerging contaminants in surface water by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry(UHPLC-Q-TOF-MS).Methods The pretreatment conditions of solid phase extraction(SPE)were op-timized by orthogonal experimental design and the surface water samples were concentrated and ex-tracted by Oasis® HLB and Oasis® MCX SPE columns in series.The extracts were separated by Kine-tex® EVO C18 column,with gradient elution of 0.1%formic acid aqueous solution and 0.1%formic acid methanol solution.Q-TOF-MS'fullscan'and'targeted MS/MS'modes were used to detect 34 emerging contaminants and to establish a database with 34 emerging contaminants precursor ion,prod-uct ion and retention times.Results The 34 emerging contaminants exhibited good linearity in the con-centration range respectively and the correlation coefficients(r)were higher than 0.97.The limit of de-tection was 0.2-10 ng/L and the recoveries were 81.2%-119.2%.The intra-day precision was 0.78%-18.70%.The method was applied to analyze multiple surface water samples and 6 emerging contaminants were detected,with a concentration range of 1.93-157.71 ng/L.Conclusion The method is simple and rapid for screening various emerging contaminants at the trace level in surface water.
关键词
法医学/毒物化学/固相萃取/超高效液相色谱-四极杆-飞行时间质谱/地表水/新兴污染物
Key words
forensic medicine/toxicology/solid phase extraction/ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry/surface water/emerging contaminants
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