In this chapter, an overview of current analytical methods, including different sample preparation techniques as well as the different instrumental approaches, is presented. The strategy literature search for the preparation of this chapter was based on the recent analytical reviews published on brominated flame retardants (BFRs), with emphasis on hexabromocyclododecane (HBCD) and tetrabromobisphenol-A (TBBPA). Additionally, we have included all new articles published in peer-reviewed scientific journals, conference proceedings, or official reports found on the internet. The analytical procedures based on the use of liquid chromatography, used for the determination of some BFRs such as TBBPA, HBCD, as well as some metabolites and transformation products are presented. Analytical performances of the different approaches (ESI, APCI, and APPI as ionization modes) are reported and compared with those obtained by gas chromatographic techniques. Conclusions and future perspectives are outlined.