High-throughput quantitation of neonicotinoids in lyophilized surface water by LC-APCI-MS/MS


Morrison, L.M., Renaud, J.B., Sabourin, L., Sumarah, M.W., Yeung, K.K.C., Lapen, D.R. (2018). High-throughput quantitation of neonicotinoids in lyophilized surface water by LC-APCI-MS/MS. Journal of AOAC International, [online] 101(6), 1940-1947. http://dx.doi.org/10.5740/jaoacint.17-0486

Plain language summary

Neonicotinoids or neonics are important insecticides used during the production of a number of crops. They are highly effective chemicals but are also controversial as there is concern about impact on bees and other organisms in environment. Their analysis is challenging for a number of reasons including the low levels that they need to be detected at. In this study we developed a method that allows for limited sample prep and easy of analysis of the 7 most important neonics in surface water.


Background: Neonicotinoids are among the most widely used insecticides. Recently, there has been concern associated with unintended adverse effects on honeybees and aquatic invertebrates at low parts-per-trillion levels. Objective: There is a need for LC-MS/MS methods that are capable of high-throughput measurements of the most widely used neonicotinoids at environmentally relevant concentrations in surface water. Methods: This method allows for quantitation of acetamiprid, clothianidin, imidacloprid, dinotefuran, nitenpyram, thiacloprid, and thiamethoxam in surface water. Deuterated internal standards are added to 20 mL environmental samples, which are concentrated by lyophilisation and reconstituted with methanol followed by acetonitrile. Results: A large variation of mean recovery efficiencies across five different surface water sampling sites within this study was observed, ranging from 45 to 74%. This demonstrated the need for labelled internal standards to compensate for these differences. Atmospheric pressure chemical ionization (APCI) performed better than electrospray ionization (ESI) with limited matrix suppression, achieving 71–110% of the laboratory fortified blank signal. Neonicotinoids were resolved on a C18 column using a 5 min LC method, in which MQL ranged between 0.93 and 4.88 ng/L. Conclusions: This method enables cost effective, accurate, and reproducible monitoring of these pesticides in the aquatic environment. Highlights: Lyophilization is used for high throughput concentration of neonicotinoids in surface water. Variations in matrix effects between samples was greatly reduced by using APCI compared with ESI. Clothianidin and thiamethoxam were detected in all samples with levels ranging from below method quantitation limit to 65 ng/L.