Determination of 83 kinds of Pharmaceuticals and Biomarkers in Wastewater via Solid Phase Extraction Coupled with Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry
10.19756/j.issn.0253-3820.231329
- VernacularTitle:固相萃取-超高效液相色谱-串联质谱法测定污水中83种药物和生物标志物
- Author:
Rui-Ling ZHANG
1
,
2
;
Xin LIU
;
Shi-Zhen ZHAO
;
Gan ZHANG
;
Peng-Ran GUO
Author Information
1. 广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广州 510070
2. 中国科学院广州地球化学研究所,有机地球化学国家重点实验室,广州 510640
- Keywords:
Pharmaceuticals;
Biomarkers;
Wastewater;
Ultra-performance liquid chromatography-tandem mass spectrometry;
Solid phase extraction
- From:
Chinese Journal of Analytical Chemistry
2024;52(8):1192-1199,中插21-中插34
- CountryChina
- Language:Chinese
-
Abstract:
Wastewater-based epidemiology(WBE)can effectively assess population health status,but it is lack of analytical methods which can simultaneously analyze a number of pharmaceuticals and biomarkers in wastewater.In this work,a method including sample pretreatment and instrumental detection for quantifying 83 kinds of pharmaceuticals and biomarkers in the influent of wastewater treatment plants(WWTPs)was established by sing solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS).The water sample(200 mL)with 83 kinds of target compounds was divided into two aliquots,which were then enriched and purified using HLB columns at pH=6.7 and pH=2 respectively,followed by elution with 6 mL of methanol and 6 mL of methanol containing 2%(V/V)formic acid,respectively,and then dried by nitrogen blown,concentrated,and finally redissolved to 0.5 mL,filtered through a nylon filter(0.22 μm).The target compounds in the samples were determined using UPLC-MS/MS in electrospray ionization under both positive and negative ion multiple reaction monitoring modes,with quantification using the internal standard method.The method exhibited good linearity(r>0.996)for the 83 kinds of target compounds in the concentration range of 0.1-500 ng/mL,and intra-day and inter-day precisions were 1.2%-16.5%.The recoveries of target substances in pure water and influent samples from a WWTP were 51.6%-166.6%and 56.4%-150.1%,respectively,with relative standard deviations of 0.2%-31.9%and 0.3%-20.9%,respectively.The method detection limits of target compounds were 0.02-7.72 ng/L.This method was applied to determine pharmaceuticals and biomarkers in the influent samples of a WWTP in Guangzhou,and 54 kinds of pharmaceuticals and 4 kinds of biomarkers were detected.The concentrations of acetaminophen and erythromycin were the highest among the pharmaceuticals,1.6-3.4 μg/L and 0.6-1.1 μg/L,respectively.The concentration of caffeine was the highest among the biomarkers,i.e.,33.3-43.9 μg/L.This method had high sensitivity,good stability and accuracy,and was suitable for detection of pharmaceuticals and biomarkers in the influent of WWTP,which could provide analytical method support for conducting studies on WBE.
