Comparative Analysis and Optimization of SFC-MS/MS and LC-MS/MS for Pesticide Residue Analysis in Bumblebee Samples
(2025) KEMR30 20251Department of Chemistry
- Abstract
- This study focuses on the chromatographic analysis of neonicotinoid pesticides in bumblebee samples. Analyzing these residues presents significant challenges due to the complex biological matrix and the critical need for high detectability to meet regulatory limits. Furthermore, many conventional chromatographic methods are often time-consuming and rely on substantial volumes of hazardous organic solvents, raising considerable environmental and operational concerns.
Two analytical methods, SFC-MS/MS and LC-MS/MS, were systematically developed and optimized. General method development for both platforms also involved rigorous column screening, mobile phase composition, and fine-tuning. For the LC-MS/MS method, Design of Experiments... (More) - This study focuses on the chromatographic analysis of neonicotinoid pesticides in bumblebee samples. Analyzing these residues presents significant challenges due to the complex biological matrix and the critical need for high detectability to meet regulatory limits. Furthermore, many conventional chromatographic methods are often time-consuming and rely on substantial volumes of hazardous organic solvents, raising considerable environmental and operational concerns.
Two analytical methods, SFC-MS/MS and LC-MS/MS, were systematically developed and optimized. General method development for both platforms also involved rigorous column screening, mobile phase composition, and fine-tuning. For the LC-MS/MS method, Design of Experiments (DoE) and Response Surface Methodology (RSM) were specifically employed to optimize the mass spectrometer's ESI ion source parameters, including sheath gas temperature, nebulizer pressure, drying gas temperature, and capillary voltage.
The optimized SFC-MS/MS method (1-AA column, back pressure gradient, methanol co-solvent gradient) demonstrated superior performance: 7 min analysis time (vs. 11 min for LC-MS/MS), higher detectability (LODs 1.2–2.4 µg/L vs. 2.64–10.75 µg/L for LC-MS/MS), and reduced organic solvent consumption (1.65 mL/run vs. 4.8 mL/run). The LC-MS/MS method (BEH Ph column) successfully detected compounds, but was less efficient.
SFC-MS/MS is a promising, greener, and more efficient alternative for high-throughput pesticide residue analysis in bumblebee matrices, offering significant advancements over traditional LC-MS/MS. (Less) - Popular Abstract
- Bumblebees are vital to our planet, but pesticides like neonicotinoids pose a serious threat to them. Detecting these chemicals accurately and at low levels is crucial; however, current laboratory methods are often time-consuming and utilize large amounts of harsh, environmentally unfriendly chemicals. My Master's research aimed to tackle this issue by developing faster, more sensitive, and greener analytical methods to detect eight of these pesticides in bumblebee samples.
We focused on optimizing two high-tech techniques: SFC-MS/MS, which uses carbon dioxide as its main carrier, and LC-MS/MS, a liquid-based separation method. Both are powerful techniques for identifying and quantifying chemicals, like fingerprinting. Our development... (More) - Bumblebees are vital to our planet, but pesticides like neonicotinoids pose a serious threat to them. Detecting these chemicals accurately and at low levels is crucial; however, current laboratory methods are often time-consuming and utilize large amounts of harsh, environmentally unfriendly chemicals. My Master's research aimed to tackle this issue by developing faster, more sensitive, and greener analytical methods to detect eight of these pesticides in bumblebee samples.
We focused on optimizing two high-tech techniques: SFC-MS/MS, which uses carbon dioxide as its main carrier, and LC-MS/MS, a liquid-based separation method. Both are powerful techniques for identifying and quantifying chemicals, like fingerprinting. Our development involved carefully selecting separation columns and fine-tuning flow rates and pressure. For LC-MS/MS, we also utilized advanced statistical tools, specifically "Design of Experiments," to determine the optimal settings for the detector source, thereby optimizing parameters such as gas temperature and voltage.
Our comparison showed that the optimized SFC-MS/MS method outperformed LC-MS/MS. It was significantly faster and more sensitive, but its major advantage was that it used substantially less organic solvent. In summary, this research successfully developed a highly efficient and environmentally responsible SFC-MS/MS method. This new approach provides better tools for environmental monitoring and also opens the door for future work to truly assess its environmental impact using specific green chemistry assessment tools. (Less)
Please use this url to cite or link to this publication:
http://lup.lub.lu.se/student-papers/record/9210766
- author
- Androutsopoulou, Theodora LU
- supervisor
- organization
- course
- KEMR30 20251
- year
- 2025
- type
- H2 - Master's Degree (Two Years)
- subject
- keywords
- Chromatography, LC-MS/MS, Neonicotinoids, Optimization, SFC-MS/MS, Analytical Chemistry
- language
- English
- id
- 9210766
- date added to LUP
- 2025-08-29 12:51:06
- date last changed
- 2025-08-29 12:51:06
@misc{9210766,
abstract = {{This study focuses on the chromatographic analysis of neonicotinoid pesticides in bumblebee samples. Analyzing these residues presents significant challenges due to the complex biological matrix and the critical need for high detectability to meet regulatory limits. Furthermore, many conventional chromatographic methods are often time-consuming and rely on substantial volumes of hazardous organic solvents, raising considerable environmental and operational concerns.
Two analytical methods, SFC-MS/MS and LC-MS/MS, were systematically developed and optimized. General method development for both platforms also involved rigorous column screening, mobile phase composition, and fine-tuning. For the LC-MS/MS method, Design of Experiments (DoE) and Response Surface Methodology (RSM) were specifically employed to optimize the mass spectrometer's ESI ion source parameters, including sheath gas temperature, nebulizer pressure, drying gas temperature, and capillary voltage.
The optimized SFC-MS/MS method (1-AA column, back pressure gradient, methanol co-solvent gradient) demonstrated superior performance: 7 min analysis time (vs. 11 min for LC-MS/MS), higher detectability (LODs 1.2–2.4 µg/L vs. 2.64–10.75 µg/L for LC-MS/MS), and reduced organic solvent consumption (1.65 mL/run vs. 4.8 mL/run). The LC-MS/MS method (BEH Ph column) successfully detected compounds, but was less efficient.
SFC-MS/MS is a promising, greener, and more efficient alternative for high-throughput pesticide residue analysis in bumblebee matrices, offering significant advancements over traditional LC-MS/MS.}},
author = {{Androutsopoulou, Theodora}},
language = {{eng}},
note = {{Student Paper}},
title = {{Comparative Analysis and Optimization of SFC-MS/MS and LC-MS/MS for Pesticide Residue Analysis in Bumblebee Samples}},
year = {{2025}},
}