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一种先进的 LC-MS/MS 协议,用于同时检测环境中的药物和个人护理产品。

An advanced LC-MS/MS protocol for simultaneous detection of pharmaceuticals and personal care products in the environment.

机构信息

Institute of Surface-Earth System Science, School of Earth System Science, Tianjin University, Tianjin, China.

Tianjin Bohai Rim Coastal Earth Critical Zone National Observation and Research Station, Tianjin University, Tianjin, China.

出版信息

Rapid Commun Mass Spectrom. 2023 Jan 15;37(1):e9397. doi: 10.1002/rcm.9397.

Abstract

RATIONALE

The development of appropriate analytical screening techniques for pharmaceuticals and personal care products (PPCPs) is the basis for studying the distribution and environmental impact of emerging contaminants (ECs). Mass spectrometry-based screening methods vary with the complexity of the target compounds. It is challenging to balance both positive and negative ion quantification with a low detection limit. To establish a set of experimental methods including extraction, chromatography-separation and mass spectrometry screening is one of the most important topics in PPCP research. This paper describes a universal and efficient qualification and quantification protocol for the simultaneous detection of 34 PPCPs in different environmental samples in a single analytical data acquisition run.

METHODS

Thirty-four representative PPCPs, which are widely distributed in the environment with high ecological toxicity and complex chemical structures, were selected as representative target ECs. The extraction of the target PPCPs was achieved using only one solid-phase extraction cartridge without the need to adjust the pH of samples. The enriched samples were detected by LC-MS/MS in both positive and negative ion modes simultaneously. The protocol was evaluated based on the accuracy, precision, detection limits and matrix effects.

RESULTS

This method achieved simultaneous detection of PPCPs in both positive and negative ion modes, with a single analytical cycle of 12 min. The observed SPE recoveries were between 40% and 115%. The instrumental detection limits (IDL) varied from 0.01 to 1 pg, and the method detection limits (MDL) were between 0.002 and 3.323 ng/l in different matrices. Most of the PPCPs were subjected to matrix suppression below 30%. The method was successfully applied for quantitative analysis of the PPCPs in different environmental samples, including river samples, wastewater treatment plant (WWTP) samples and soil samples.

CONCLUSIONS

This protocol developed a rapid and efficient detection method to simultaneous qualitative and quantitative 34 representative PPCPs in the environment. The IDL ranged from 0.01 to 1 pg and the MDL ranged from 0.002 to 3.323 ng/l in different matrices. The detection limit was one order of magnitude lower compared to previous studies. The protocol also provided a wide application range for different environmental matrices, which permitted the migration and transformation of PPCPs to be explored.

摘要

原理

开发适当的分析筛选技术来检测药品和个人护理产品(PPCPs)是研究新兴污染物(ECs)分布和环境影响的基础。基于质谱的筛选方法因目标化合物的复杂性而异。平衡正负离子定量和低检测限具有挑战性。建立一套包括提取、色谱分离和质谱筛选的实验方法是 PPCP 研究中最重要的课题之一。本文描述了一种通用且高效的定性和定量方法,可在单次分析数据采集运行中同时检测不同环境样品中的 34 种 PPCPs。

方法

选择 34 种具有代表性的 PPCPs,这些 PPCPs广泛分布于环境中,具有高生态毒性和复杂的化学结构,作为代表性目标 ECs。目标 PPCPs 的提取仅使用一个固相萃取小柱即可完成,无需调整样品的 pH 值。富集后的样品通过 LC-MS/MS 在正负离子模式下同时检测。该方案基于准确性、精密度、检测限和基质效应进行评估。

结果

该方法实现了 PPCPs 在正负离子模式下的同时检测,单个分析周期为 12 分钟。观察到的 SPE 回收率在 40%至 115%之间。仪器检测限(IDL)在不同基质中从 0.01 至 1 pg 不等,方法检测限(MDL)在不同基质中从 0.002 至 3.323 ng/l 不等。大多数 PPCPs 的基质抑制低于 30%。该方法成功应用于不同环境样品中 PPCPs 的定量分析,包括河流样品、污水处理厂(WWTP)样品和土壤样品。

结论

本研究开发了一种快速有效的检测方法,可同时定性和定量检测环境中 34 种具有代表性的 PPCPs。IDL 在不同基质中从 0.01 至 1 pg 不等,MDL 在不同基质中从 0.002 至 3.323 ng/l 不等。与之前的研究相比,检测限低了一个数量级。该方案还为不同的环境基质提供了广泛的应用范围,允许探索 PPCPs 的迁移和转化。

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