Determination of Acetamiprid by HPLC-Fluorescence With Post-Column Photoderivatization and HPLC-Mass Selective Detection

Abstract

Two methods are described for determining the highly polar pesticide acetamiprid in vegetables. Residues are extracted with ethyl acetate and coextratives are removed with a graphitised Carbon-based packing ENVI-carb cartridge. Analysis is performed with goods results, by HPLC with post-column photoderivatization, and fluorescence detection and by HPLC-Electrospray ionisation mass spectrometry. The clean-up step is not necessary in this last case. LODs were 6 mg L À1 for HPLCfluorescence detection using matrix matched standards and 1.5 mg L À1 for HPLC-ES-MS detection. Recovery data were obtained by fortifying vegetable matrix at 0.01, 0.1, and 0.5 mg kg À1 , with recoveries between 65 and 75% for the HPLC-fluorescence and between 72 and 77% for HPLC-ES-MS.

Simultaneous determination of acetamiprid and 6‐chloronicotinic acid in environmental samples by using ion chromatography hyphenated to online photoinduced fluorescence detector

“…It was found that ATP exhibited high PIF signal intensity at λ ex /λ em = 257/382 nm, while its metabolite 6‐CNA shown the high PIF intensity at λ ex /λ em = 231/370 nm. These calculated wavelengths appeared approximately the same as previously reported [12,21]. Hence, the fluorescence detector was programmed at λ ex /λ em = 257/382 nm for ATP up to 6.0 min, while λ ex /λ em = 231/370 nm was set for 6‐CNA for the rest of the analysis time.…”

“…But its successful application is impeded by poor selectivity and sensitivity of UV detector for the accurate quantification of neonicotinoids in the sample matrices [6,7,12,19,20]. LC coupled with a fluorescence detector (LC‐FLD) is a comparatively simple, cost‐effective, sensitive, and selective technique for the high‐throughput and accurate quantification of analytes of interest [21]. Although, its direct application is restricted by the intrinsic nonfluorescent characteristic of neonicotinoids including ATP and its metabolite 6‐CNA.…”