A simple analytical method was developed for the determination of total bromine in fruits and grain products by means of wavelength dispersive X-ray fluorescence spectrometry (WDXRF). Five gram samples of fresh fruits, frozen fruits, dried fruits and grain products were extracted with distilled water twice and diluted to 25 mL with distilled water. The sample solution (0.5 mL) was dripped onto the filter paper, which was dried and analyzed by WDXRF. The working curve was linear in the range of 0 to 10 μg/mL. Recoveries at the level of 5 μg/g were 76-104%. The detection limit was 0.5 μg/g and the determination limit was 1.5 μg/g in foods. Compared to the GC-ECD method, this method gave equivalent results for fresh fruits, frozen fruits and grain products. In addition, some dried fruits, in which a slightly high level was detected, gave almost the same results with the GC-ECD method. Therefore, this method is considered to be available as an alternative to the GC-ECD method.
A novel multi-functional adsorbent (RP-SAX adsorbent) bearing hydrophobic and anion exchange groups was synthesized for the simple and rapid determination of residual acephate (AP) in vegetables. Macroporous base resin was obtained by suspension copolymerization with glycidyl methacrylate, stearyl methacrylate and glycerin dimethacrylate, and then ethyldimethylamine was introduced at glycidyl groups on the base resin. The adsorbent was packed into a syringe-type tube and used for extraction of AP. AP in the vegetable extract was quantitatively entrapped on the adsorbent and was completely eluted with 3 mL of 30 mmol/L trisodium phosphate in 50% (v/v) methanol solution. The eluate was directly injected into an HPLC-UV detection system with a reverse-phased column. The recoveries of 5 mg/L AP spiked in vegetable extraction samples ranged from 77% to 100%.
A real-time polymerase chain reaction (PCR) method specific for genetically modified (GM) maize event DAS59132 (E32) was adapted for qualitative detection of low level presence of E32. The method was validated by a collaborative trial with eight participating Japanese laboratories. Sensitivity was assessed with three different samples of corn flour fortified to 0%, 0.05% and 0.1% (w/w) E32 respectively. In addition, a 0.01% E32 DNA solution was used. The detection limit with DNA solution was estimated to be approximately 0.01%. In conclusion, the results of the study confirmed this real-time PCR method as a reliable tool for qualitative detection of E32 maize.