Environmentally friendly analysis of sulphonamides in Brazilian honey through automated and miniaturised sample preparation coupled with LC-MS/MS

Abstract

Increased use of environmentally friendly practices has become a trend in science because of the current awareness regarding climate change and related issues. Similarly for analytical chemistry, considering the development of greener methods for reducing the use of reagents and samples and also toxic waste generation. To meet such goals, automation, and miniaturisation of sample preparation-a well-recognised laborious and time-consuming analytical step-are two promising strategies. This work associates the greener aspects of miniaturisation and the performance of automated sample preparation. Therefore, we proposed an analytical method using a miniaturised extraction column for pre-concentrating sulphamerazine, sulphamethazine, sulphamethoxazole, sulphadimethoxine, sulphathiazole, and sulphachlorpyridazine from honey and cleaning-up the samples. Several variables were optimised: extractive phase, loading flow, loading phase, and loading time. Under optimised conditions, the method showed adequate linearity between 5.0 and 60 ng g^-1 with R > 0.99, and also good selectivity and recovery (114.6-124.1%) which are acceptable according to Brazilian legislation. Intra and inter-day precision were in the range 3.0-5.0%. Although sulphonamides were detected in one of the eight commercial honey samples, the value was below the established MRL. The method showed efficiency, while also exhibiting greener characteristics resulting from miniaturisation and automation, representing a promising environmentally friendly alternative for conventional sample preparation methods.

Keywords: Honey; automation; liquid chromatography; mass spectrometry; miniaturization; sulphonamides.