Determination, residue and risk assessment of trifloxystrobin, trifloxystrobin acid and tebuconazole in Chinese rice consumption.

A simple and rapid analytical method for the detection of trifloxystrobin, trifloxystrobin acid and tebuconazole in soil, brown rice, paddy plants and rice hulls was established and validated by liquid chromatography with tandem mass spectrometry. Acceptable linearity (R2 > 0.99), accuracy (average recoveries of 74.3-108.5%) and precision (intra- and inter-day relative standard deviations of 0.9-8.8%) were obtained using the developed determination approach. In the field trial, the half-lives of trifloxystrobin and tebuconazole in paddy plants were 5.7-8.3 days in three locations throughout China, and the terminal residue concentrations of trifloxystrobin and tebuconazole were <100 and 500 µg/kg (maximum residue limits set by China), respectively, at harvest, which indicated that, based on the recommended application procedure, trifloxystrobin and tebuconazole are safe for use on rice. The risk assessment results demonstrated that, owing to risk quotient values of both fungicides being <100%, the potential risk of trifloxystrobin and tebuconazole on rice was acceptable for Chinese consumers. These data could provide supporting information for the proper use and safety evaluation of trifloxystrobin and tebuconazole in rice.

Persistence, dissipation, and risk assessment of a combination formulation of trifloxystrobin and tebuconazole fungicides in/on tomato.

Multi-locational supervised field trials were conducted in different agro-climatic regions in India to study dissipation of trifloxystrobin and tebuconazole in tomato after spraying a combination formulation (trifloxystrobin 25% + tebuconazole 50%, 75WG) at recommended doses: (i) single (trifloxystrobin 87.5 g a.i. ha-1 + tebuconazole 175 g a.i. ha-1) and (ii) double (trifloxystrobin 175 g a.i. ha-1 + tebuconazole 350 g a.i. ha-1). Fruit samples were extracted with ethyl acetate using a modified QuEChERS method. The residues (parent fungicides + metabolite) were analyzed and confirmed by GC-ECD and GC-MS, respectively. The half-life (t1/2) of trifloxystrobin and tebuconazole in tomato varied from 1.08 to 1.72 and 1.13 -to 1.64 days at single; and 1.27 to 2.13 and 1.24 to 1.96 days at double dose, respectively. Since maximum residue limit (MRL) at pre-harvest interval (PHI) of 5 days is impractical, as tomato is usually harvested and consumed almost everyday after the last spray, the risk assessment was performed at minimum PHI of 1 day. Accordingly, on the basis of supervised field trial data and using OECD MRL calculator, MRL of 0.5 and 1.5 mg kg-1 at single dose were proposed for trifloxystrobin and tebuconazole in/on tomato, respectively.

Occurrence of cyclic imines in European commercial seafood and consumers risk assessment.

Cyclic imines constitute a quite recently discovered group of marine biotoxins that act on neural receptors and that bioaccumulate in seafood. They are grouped together due to the imino group functioning as their common pharmacore, responsible for acute neurotoxicity in mice. Cyclic imines (CIs) have not been linked yet to human poisoning and are not regulated in the European Union (EU), although the European Food Safety Authority (EFSA) requires more data to perform conclusive risk assessment for consumers. Several commercial samples of bivalves including raw and processed samples from eight countries (Italy, Portugal, Slovenia, Spain, Ireland, Norway, The Netherlands and Denmark) were obtained over 2 years. Emerging cyclic imine concentrations in all the samples were analysed on a LC-3200QTRAP and LC-HRMS QExactive mass spectrometer. In shellfish, two CIs, pinnatoxin G (PnTX-G) and 13-desmethylspirolide C (SPX-1) were found at low concentrations (0.1-12µg/kg PnTX-G and 26-66µg/kg SPX-1), while gymnodimines and pteriatoxins were not detected in commercial (raw and processed) samples. In summary, SPX-1 (n: 47) and PnTX-G (n: 96) were detected in 9.4% and 4.2% of the samples, respectively, at concentrations higher than the limit of quantification (LOQ), and in 7.3% and 31.2% of the samples at concentrations lower than the LOQ (25µg/kg for SPX-1 and 3µg/kg for PnTX-G), respectively. For the detected cyclic imines, the average exposure and the 95th percentile were calculated. The results obtained indicate that it is unlikely that a potential health risk exists through the seafood diet for CIs in the EU. However, further information about CIs is necessary in order to perform a conclusive risk assessment.

Simultaneous determination of trifloxystrobin and trifloxystrobin acid residue in rice and soil by a modified quick, easy, cheap, effective, rugged, and safe method using ultra high performance liquid chromatography with tandem mass spectrometry.

A sensitive analytical method for the simultaneous determination of trifloxystrobin and its metabolite trifloxystrobin acid in rice including straw, bran, brown rice and soil was developed by using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The fungicide trifloxystrobin and its metabolite trifloxystrobin acid were extracted using acetonitrile with 1% formic acid v/v and subsequently cleaned up by primary secondary amine, octadecylsilane or graphitized carbon black prior to ultra high performance liquid chromatography coupled with tandem mass spectrometry. The determination of two target compounds was achieved in less than 3 min using an electrospray ionization source in positive mode. The limits of detection were below 0.22 µg/kg and the limits of quantification did not exceed 0.74 µg/kg in all matrices, which were much lower than the maximum residue levels established by the Codex Alimentarius Commission. The overall average recoveries in four matrix at three levels (0.1, 1.0 and 5.0 mg/kg) ranged from 74.2 to 107.4% with a relative standard deviations of less than 7.8% (n = 5) for both analytes. The method was demonstrated to be convenient and reliable for the routine monitoring of trifloxystrobin and its metabolite. The developed method was validated and applied for the analysis of degradation study samples.