首页|地表水中34种新兴污染物的超高效液相色谱-四极杆-飞行时间质谱快速筛查

地表水中34种新兴污染物的超高效液相色谱-四极杆-飞行时间质谱快速筛查

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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.
Rapid Screening of 34 Emerging Contaminants in Surface Water by UHPLC-Q-TOF-MS
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.

forensic medicinetoxicologysolid phase extractionultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometrysurface wateremerging contaminants

吕琛山、曹艺璇、穆哓茜、崔海燕、王涛、尉志文、贠克明、胡萌

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山西医科大学法医学院,山西 晋中 030600

法医学山西省重点实验室,山西 晋中 030600

法庭毒物分析公安部重点实验室,山西 晋中 030600

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

国家自然科学基金资助项目国家自然科学基金资助项目国家自然科学基金资助项目国家重点研发计划资助项目国家重点研发计划资助项目

2180609582130056820721162017YFC08035042018YFC0807403

2024

10.12116/j.issn.1004-5619.2022.320301

法医学杂志
司法部司法鉴定科学技术研究所

法医学杂志

CSTPCDCHSSCD北大核心
影响因子：0.32
ISSN：1004-5619
年,卷(期)：2024.40(1)
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