PBDEs are widely used brominated flame retardant, which are increasingly reported in the environment. Concentrations of thirteen PBDEs in a large number of channel catfish and fish feeds collected from Hubei province ...PBDEs are widely used brominated flame retardant, which are increasingly reported in the environment. Concentrations of thirteen PBDEs in a large number of channel catfish and fish feeds collected from Hubei province of China were investigated in this study. A fast isotopic dilution GC-MS method was firstly developed to simultaneously determine thirteen PBDEs in channel catfish and fish feeds in this study, and especially for the first time PBDEs in fish feeds. Pressurized liquid extraction and multi-layer silica gel column chromatography cleanup were used, some important steps and crucial parameters were modified and intensified compared with other literatures, and GC and MS conditions were optimized. The limits of quantitation values of 0.25 - 5 μg·kg-1 wet weight in channel catfish were calculated for PBDEs;so did 1 - 20 μg·kg-1 wet weight in fish feeds. In addition, good repeatability and accuracy of the whole method were achieved. The established methods were therefore suitable for the simultaneous determinations of thirteen PBDEs in these samples at trace contamination levels. Using the established methods, PBDEs emerged in 10 of 180 channel catfish and 13 of 115 fish feeds, and the dominant PBDEs homologues were PBDE-28, PBDE-47, PBDE-100, PBDE-99, PBDE-154, PBDE-153 and PBDE-183. The detection rates of seven PBDEs congeners were in turn respectively 1.74%, 7.83%, 4.35%, 5.22%, 3.48%, 2.61% and 2.61% in fish feeds, and detection rates of seven PBDEs congeners were in turn respectively 1.11%, 3.89%, 2.22%, 1.67%, 1.11%, 1.11% and 1.11% in channel catfish. There was significant correlation in PBDEs between matching channel catfish and fish feeds (R2 = 0.742, P < 0.001, n = 30), suggesting that fish feeds contaminated with PBDEs possibly resulted in PBDEs residual in channel catfish through biological transfer.展开更多
文摘PBDEs are widely used brominated flame retardant, which are increasingly reported in the environment. Concentrations of thirteen PBDEs in a large number of channel catfish and fish feeds collected from Hubei province of China were investigated in this study. A fast isotopic dilution GC-MS method was firstly developed to simultaneously determine thirteen PBDEs in channel catfish and fish feeds in this study, and especially for the first time PBDEs in fish feeds. Pressurized liquid extraction and multi-layer silica gel column chromatography cleanup were used, some important steps and crucial parameters were modified and intensified compared with other literatures, and GC and MS conditions were optimized. The limits of quantitation values of 0.25 - 5 μg·kg-1 wet weight in channel catfish were calculated for PBDEs;so did 1 - 20 μg·kg-1 wet weight in fish feeds. In addition, good repeatability and accuracy of the whole method were achieved. The established methods were therefore suitable for the simultaneous determinations of thirteen PBDEs in these samples at trace contamination levels. Using the established methods, PBDEs emerged in 10 of 180 channel catfish and 13 of 115 fish feeds, and the dominant PBDEs homologues were PBDE-28, PBDE-47, PBDE-100, PBDE-99, PBDE-154, PBDE-153 and PBDE-183. The detection rates of seven PBDEs congeners were in turn respectively 1.74%, 7.83%, 4.35%, 5.22%, 3.48%, 2.61% and 2.61% in fish feeds, and detection rates of seven PBDEs congeners were in turn respectively 1.11%, 3.89%, 2.22%, 1.67%, 1.11%, 1.11% and 1.11% in channel catfish. There was significant correlation in PBDEs between matching channel catfish and fish feeds (R2 = 0.742, P < 0.001, n = 30), suggesting that fish feeds contaminated with PBDEs possibly resulted in PBDEs residual in channel catfish through biological transfer.