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Fully-automated SPE coupled to UHPLC-MS/MS method for multiresidue analysis of 26 trace antibiotics in environmental waters: SPE optimization and method validation
- Source :
- Environmental Science and Pollution Research. 29:16973-16987
- Publication Year :
- 2021
- Publisher :
- Springer Science and Business Media LLC, 2021.
-
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.
- Subjects :
- Detection limit
Analyte
Chromatography
Chemistry
Elution
Health, Toxicology and Mutagenesis
Solid Phase Extraction
Water
General Medicine
Pollution
Anti-Bacterial Agents
Wastewater
Tandem Mass Spectrometry
Liquid chromatography–mass spectrometry
Environmental Chemistry
Sample preparation
Solid phase extraction
Effluent
Chromatography, High Pressure Liquid
Water Pollutants, Chemical
Subjects
Details
- ISSN :
- 16147499 and 09441344
- Volume :
- 29
- Database :
- OpenAIRE
- Journal :
- Environmental Science and Pollution Research
- Accession number :
- edsair.doi.dedup.....2c72c61b8d479c828ed18851be1f54c9