Improved Approach for Analyzing Bromophenols in Seafood Using Stable Isotope Dilution Analysis in Combination with SPME

An analytical method for the measurement of five naturally occurring bromophenols of sensory relevance in seafood (barramundi and prawns) is presented. The method combines simultaneous distillation−extraction followed by alkaline back extraction of a hexane extract and subsequent acetylation of the bromophenols. Analysis of the bromophenol acetates was accomplished by headspace solid phase microextraction and gas chromatography−mass spectrometry using selected ion monitoring. The addition of 13C6 bromophenol stable isotope internal standards for each of the five congeners studied permitted the accurate quantitation of 2-bromophenol, 4-bromophenol, 2,6-dibromophenol, 2,4-dibromophenol, and 2,4,6-tribromophenol down to a limit of quantification of 0.05 ng/g of fish flesh. The method indicated acceptable precision and repeatability and excellent linearity over the typical concentration range of these compounds in seafood (0.5−50 ng/g). The analytical method was applied to determine the concentration of bromophenols in a range of farmed and wild barramundi and prawns and was also used to monitor bromophenol uptake in a pilot feeding trial.

Testing insecticides against Phthorimaea operculella (Zeller) (Lepidoptera: Gelechiidae) using a tomato plant bioassay

A bioassay technique was developed to test the efficacy of insecticides against potato moth (Phthorimaea operculella (Zeller)) on tomatoes. The technique tested efficacy against both larvae in mines and neonate larvae that had not yet penetrated the leaf, and explained the failure of some insecticides to control P. operculella infestations in commercial tomato crops. Neonate larvae placed on leaves of potted plants several days before treatment provided larvae for testing of insecticides against larvae in mines; other neonates were placed on leaves after treatment to test efficacy against larvae yet to penetrate the leaf. The plants were sprayed with the candidate insecticides, held for 5-7 days, and larval mortality assessed. Chlorfenapyr (100, 200 g a.i. ha-1) and abamectin (8.1 g a.i. ha-1) were effective against neonate larvae and larvae in mines. Sulprofos (720 g a.i. ha -1), methomyl (450 g a.i. ha-1) and spinosad (96 g a.i. ha-1) were effective against neonate larvae but not against larvae in mines. Methamidophos (1102 g a.i. ha-1), endosulfan (700 g a.i. ha-1) and Bacillus thuringiensis kurstaki (1000 g ha-1) had some effect against exposed larvae but little against larvae in mines. Thiodicarb (525 g a.i. ha-1), azinphos-ethyl (440 g a.i. ha -1), imidacloprid (59.5 g a.i. ha-1), hexaflumuron (50 g a.i. ha-1), methoxyfenozide (300 g a.i. ha-1) and tebufenozide (200 g a.i. ha-1) were ineffective. A field trial using chlorfenapyr (25, 50, 100, 150 and 200 g a.i. ha-1) and methamidophos (1102 g a.i. ha-1) validated the bioassay technique, with chlorfenapyr effective in reducing the numbers of larvae in mines in leaves.