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This chapter summarizes methods and experimental approaches involved in the study of glucuronidation of several naturally occurring metabolites of the free fatty acids (FFAs), linoleic acid (LA), and arachidonic acid (AA). Data on FA glucuronidation from both human liver micro-somes and human recombinant UDP-glucuronosyltransferase 2B7 (UGT2B7) are presented. Several unique methods for synthesis of FAs that are not commercially available are also described. Moreover, comprehensive methods for measurements of FA glucuronidation, isolation of biosynthesized glucuronides, and analysis by HPLC, HPLC-MS, and GC-MS are discussed in detail. The enzymatic assays presented in this chapter can also be used for studying glucuronidation of other hydrophobic endogenous compounds, including many drugs and environmental pollutants. The potential value of these methods is highlighted by the growing appreciation of the roles of FFA and FA-glucuronides in human health and disease. [ABSTRACT FROM AUTHOR]