Fully-automated SPE coupled to UHPLC-MS/MS method for multiresidue analysis of 26 trace antibiotics in environmental waters: SPE optimization and method validation

Ming Zheng; Suwen Tang; Yangyang Bao; Kevin D Daniels; Zuo Tong How; Mohamed Gamal El-Din; Jie Wang; Liang Tang

doi:10.1007/s11356-021-15947-3

Fully-automated SPE coupled to UHPLC-MS/MS method for multiresidue analysis of 26 trace antibiotics in environmental waters: SPE optimization and method validation

Environ Sci Pollut Res Int. 2022 Mar;29(12):16973-16987. doi: 10.1007/s11356-021-15947-3. Epub 2021 Oct 16.

Authors

Ming Zheng^#¹, Suwen Tang^#², Yangyang Bao³, Kevin D Daniels⁴, Zuo Tong How⁵, Mohamed Gamal El-Din⁵, Jie Wang⁶, Liang Tang⁷

Affiliations

¹ Key Laboratory of Organic Compound Pollution Control Engineering, School of Environmental and Chemical Engineering, Shanghai University, Shanghai, 200444, China. zmshu@shu.edu.cn.
² Key Laboratory of Organic Compound Pollution Control Engineering, School of Environmental and Chemical Engineering, Shanghai University, Shanghai, 200444, China.
³ Pudong New Area Environmental Monitoring Station, No.51 Lingshan Road. Pudong New Area, Shanghai, China.
⁴ Hazen and Sawyer, 1400 E. Southern Ave, Tempe, AZ, 85282, USA.
⁵ Department of Civil & Environmental Engineering, University of Alberta, Edmonton, Alberta, T6G 1H9, Canada.
⁶ Fishery Machinery and Instrument Research Institute of Chinese Academy of Fishery Sciences, Shanghai, China.
⁷ Key Laboratory of Organic Compound Pollution Control Engineering, School of Environmental and Chemical Engineering, Shanghai University, Shanghai, 200444, China. tang1liang@shu.edu.cn.

^# Contributed equally.

PMID: 34657257
DOI: 10.1007/s11356-021-15947-3

Abstract

Achieving simultaneous determination of antibiotic multiresidues in environmental waters by solid phase extraction (SPE) coupled with ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with detection limits ≤ ng L^-1 is still a huge challenge. Moreover, the offline SPE procedure was performed manually, costly, and time-consuming, while the online SPE required precision pretreatment instruments that require highly-skilled personnel. In this paper, a fully automated SPE coupled with UHPLC-MS/MS method was developed for analysis of antibiotics (sulfonamides, quinolones, and macrolides) in water matrices. Sample preparation optimization included SPE materials and configuration (HLB disks), sample volume (500-1000 mL), and pH (pH = 3) with a flow rate at 2~5 mL min^-1, and an elution procedure with 2 × 6 mL methanol, and 2 × 6 mL acetone. Meanwhile, the parameters for UHPLC-MS/S detection of analytes were optimized, including LC retention time, and MS parameters. The instrumental limits of detection (LOD) and quantification (LOQ) of analytes ranged from 0.01-0.72 μg L^-1 and 0.05-2.39 μg L^-1, respectively, with satisfactory linear calibration (R² > 0.995) and precision (< 9.9%). Recoveries in spike samples ranged between 77.5-104.9% in pure water, 59.4-97.8% in surface water (SW), and 58.2-108.6% in wastewater effluent (WWE) with relative standard deviations ≤ 12.8%. The matrix effects observed for most analytes were suppression (0-28.1%) except for five analytes having presented enhancement (0-14.6 %) in SW or WWE. This method can basically meet the needs of trace antibiotic residues detection in waters, with examples of concentrations of detected antibiotics being lower than LOQ (LLQ) -94.47 ng L^-1 in WWEs and LLQ-15.47 ng L^-1 in SW in the lower reaches of the Yangtze River Basin.

Keywords: Environmental water samples; SPE optimization; Sulfonamide, quinolone, and macrolide antibiotics; UHPLC–MS/MS; Validation.

MeSH terms

Anti-Bacterial Agents
Chromatography, High Pressure Liquid
Solid Phase Extraction
Tandem Mass Spectrometry*
Water
Water Pollutants, Chemical*

Substances

Anti-Bacterial Agents
Water Pollutants, Chemical
Water

Abstract

MeSH terms

Substances

Grants and funding