Optimization of the method for analysing neonicotinoids and their metabolites in hoverflies using supercritical fluid extraction and liquid chromatography coupled to triple quadruple mass spectrometer

Abstract

The extensive use of neonicotinoids has raised concerns about their impact on pollinators like hoverflies, which are vital for pollination and ecosystem health. This study develops and validates a green extraction method using Supercritical Fluid Extraction (SFE), coupled with HPLC (High Performance Liquid Chromatography) - MS/MS (Mass Spectrometry) for selective analysis.

SFE was employed as a more environmentally friendly technique to extract neonicotinoids and their metabolites from hoverfly samples, minimizing solvent use and reducing environmental impact. The HPLC-MS/MS system enabled sensitive and selective detection of several neonicotinoids and metabolites.

The method met SANTE 11312/2021 validation criteria, showing good linearity (R ≥ 0.99), precision (RSD < 5%), and acceptable recoveries (35–95%) at 200–400 ppb. Matrix effects were low to moderate (<±20%). Greenness was evaluated using the Eco-Scale and Analytical Greenness Score. This SFE-LC-MS/MS method offers a sustainable tool for monitoring pesticide residues in pollinators and supports research on their environmental impact.

Popular Abstract

Pollinators, such as bees and hoverflies, are essential for food and ecosystems. Without them, many fruits, vegetables, and wild plants would struggle to grow. Unfortunately, the use of pesticides, especially a group called neonicotinoids, in farming is suspected to harm these insects. But the question is how much of these chemicals do pollinators really carry in their tiny bodies.

The goal of this study was to better understand the number of pesticides and their breakdown products (metabolites) present in insects exposed to them. To do this, I worked with samples of hoverflies, important pollinators in Europe, and developed a method to extract and measure pesticides from their bodies.

To get these substances out of the insects in a safe environmental and efficient way, I used a technique called Supercritical Fluid Extraction, which works a bit like a powerful but gentle chemical vacuum cleaner. Then, to detect and measure the pesticides, I used high-performance liquid chromatography with mass spectrometry, which is a very sensitive tool often used in advanced chemical analysis.

One of the biggest challenges is finding the correct conditions to extract the chemicals without damaging the samples or clogging the system. After several tests, I found that a combination of carbon dioxide and acetonitrile (a type of solvent) worked best. I also compared other common solvents, like ethanol and methanol, and found that even though ethanol is a greener option, acetonitrile gave better results.

The results showed that residues of certain pesticides and their breakdown products could be detected in the insects, proving that these compounds can stay inside the pollinators for some time. This work provides useful insights for environmental monitoring and can support future decisions about pesticide use in agriculture.

In short, this project shows how chemical analysis can help protect pollinators, tiny creatures with a big impact on the health of our planet.

• author: Quintana Melian, Maria
• supervisor: Fiona Maungo Nermark; Mona Fathi
• organization: Department of Chemistry
• course: KEMR30 20251
• year: 2025
• type: H2 - Master's Degree (Two Years)
• subject: Chemistry
• keywords: analytical chemistry, hoverflies, metabolites, neonicotinoids, HPLC-MS/MS: SFE
• language: English
• id: 9212981
• date added to LUP: 2025-09-24 09:11:02
• date last changed: 2025-09-24 09:11:02