Semiautomated determination of neonicotinoids and characteristic metabolite in urine samples using TurboFlow™ coupled to ultra high performance liquid chromatography coupled to Orbitrap analyzer

• Published in: Journal of pharmaceutical and biomedical analysis 2017-11, Vol.146, p.378-386
• Main Authors: López-García, Marina, Romero-González, Roberto, Lacasaña, Marina, Garrido Frenich, Antonia
• Format: Article
• Language: English
• Subjects: Chromatography, High Pressure Liquid - methods; Female; Humans; Insecticides - chemistry; Insecticides - urine; Limit of Detection; Metabolite; Neonicotinoids; Neonicotinoids - chemistry; Neonicotinoids - urine; Online SPE; Orbitrap; Pregnancy; Reproducibility of Results; Solid Phase Extraction - methods; Spain; Tandem Mass Spectrometry - methods; TurboFlow; Urine; Urine - chemistry
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2017.08.026

[Display omitted] •Seven neonicotinoids and one metabolite have been determined by LC-Orbitrap.•Two online extraction systems were evaluated: TurboFlow™ and SPE.•Thirty six urine samples were analyzed by the developed method.•Three neonicotinoids and one metabolite were detected in urine samples. A semiautomated method based on ultra-high performance liquid chromatography (UHPLC) coupled to Orbitrap high resolution mass spectrometry has been developed for the determination of neonicotinoids (imidacloprid, acetamiprid, clothianidin, dinotefuran, nitenpyram, thiacloprid and thiamethoxam) and the metabolite acetamiprid-n-desmethyl in urine samples. Two automated methods were tested (solid-phase extraction “SPE” and turbulent flow chromatography “TurboFlow™”), obtaining the best results when TurboFlow™ was applied. The total analysis time for the developed method was 14min. The optimized method was validated, obtaining suitable results for all validation parameters. Recoveries ranged from 78% to 116% meanwhile repeatability and reproducibility were evaluated obtaining values lower than 10% and 20% respectively (except for dinotefuran and nitenpyram at 0.2μgL−1). The limit of quantification (LOQ) for all compounds was established at 0.2μgL−1. The proposed analytical methodology was applied to analyze the target compounds in thirty six urine samples from pregnant women living in agricultural areas of Almería (Spain). Imidacloprid, acetamiprid and acetamiprid-n-desmethyl were detected in some of the samples at concentrations ranging from 0.23 to 1.57μgL−1. Furthermore, dinotefuran was identified in two samples at trace levels.