基于超高效液相色谱-高分辨质谱技术的水中112种药品和个人护理用品的高通量筛查和定量方法

采用超高效液相色谱-三重四极杆/静电场轨道阱高分辨质谱法（UHPLC-Q-Orbitrap MS），建立了水中112种药品和个人护理用品类污染物（PPCPs）的快速筛查及定量分析方法。水样分别在酸性及碱性条件下提取，分别经SPE柱净化，以UHPLC-Q-Orbitrap MS进行分离检测，采用全扫描/数据依赖二级扫描（Full MS/dd-MS²）模式进行扫描，实现了水中112种PPCPs的定性筛查，并基于一级母离子峰面积对其含量进行了定量检测。112种PPCPs的定量限为0.002~0.8 μg/L，在各自的线性范围内均呈良好的线性关系（r²≥0.9901）； 3个水平（0.2、0.4、0.8 μg/L）下的添加回收率为60.1%~129.5%，相对标准偏差为1.1%~17.8%（n=6）。将所建立的方法用于来自大连市7个区的水样中PPCPs的筛查，共筛查出16种污染物，并对其进行了定量分析。本方法简单快速，灵敏度高，筛查范围广，为水质的管理和环境风险监测提供了一种有力的技术手段。

High-throughput screening and quantitative analysis method of 112 pharmaceutical and personal care products in water based on ultra-high performance liquid chromatography with high-resolution mass spectrometry

An effective method based on ultra-high performance liquid chromatography-triple quadrupole/electrostatic field orbitrap mass spectrometry (UHPLC-Q-Orbitrap MS) was developed for high-throughput screening and quantitative analysis of 112 pharmaceutical and personal care products (PPCPs) in water. The water samples were separately extracted under alkaline and acidic conditions and cleaned on an SPE column (Cleanert PEP-2). The sample was separated and detected by UHPLC-Q-Orbitrap MS, and the data were collected in full MS scan/date dependent MS2 mode. All the 112 PPCPs in water were qualitatively screened and quantified on the basis of the peak area of the precursor ion. The PPCPs showed a good linear response in the mass concentration range of three orders of magnitude (r² ≥ 0.9901), and the limits of quantification were between 0.002 μg/L and 0.8 μg/L. The recoveries of 60.1%-129.5% were achieved at different spiked levels of 0.2, 0.4, and 0.8 μg/L, and the RSDs were 1.1%-17.8% (n=6). Moreover, the method was used to screen the PPCPs in water samples acquired from seven regions of Dalian city (China), and 16 PPCPs were identified and quantified. Therefore, this simple method with high sensitivity and wide screening range can be applied to water quality management and environmental risk monitoring.