Optimization and standardization of GC-muECD method for the low level determination of seven polybrominated diphenyl ethers (PBDEs) found in serum sample

This study reports an efficient method for the determination of seven polybrominated diphenyl ethers (PBDEs) using GC-muECD in serum matrices. Polybrominated diphenyl ethers (PBDEs) belong to the category of brominated flame retardants commonly used in electronics, furniture and clothing. The increase in the levels of PBDEs in humans and their toxic effects in animal models attracted the attention of scientists across the globe and encouraged them to design techniques for their analysis. The need to develop an analytical method for the quantitative determination of PBDEs was important because these compounds have a high spanning concentration range (0-450 ng/ml) and predominant and widely disseminated in environmental matrix. Three different solvents [hexane, hexane/dichloro methane (60:40 v/v) and hexane/acetone (60:40 v/v)] using Accelerated solvent extraction (ASE) were compared and present standard operating procedure (SOP) for the analysis of PCBs was modified, so that its applicability can also be extended for the quantitative determination of PBDEs. There is a significant difference in the % mean recovery between all the three different solvents when paired two sample t-test for means was performed. The consistency in terms of % mean recovery, steady and smooth chromatograms and error bars also indicates that hexane is more efficient than the other two systems. The modified method was practical with respect to linearity (r 2=0.99) and had a wide range of linearity (0.06-30 ng/ml), good precision (less than 8%) and accuracy (less than 11%). The MDL and MQL calculated for this method was ≤ 0.053 ng/ml and ≤ 0.188 ng/ml respectively. These low detection limits and good recovery values (85-121%) at QC spike level of 1.0 ng/ml and 2.5 ng/ml also suggests that the applicability of this method for the analysis of PBDEs in serum samples.