Extracting OMCs from environmental samples is extremely complex because of two competing factors: achieving sufficient recovery and preventing losses, particularly the degradation of the chemicals or compounds. The recoveries and the assessment of extraction techniques for OMCs are documented in this chapter. A wide advances in analytical methods and all the latest discoveries in this field are discussed. This chapter intends to summarize the most recent approaches and techniques discovered for improving the reliability of speciation analysis of OMCs. Numerous environmental and biological studies recommend derivatization procedures for the determination of OTCs. A focus on hydride generation, alkylation by GRs, and ethylation with sodium tetraethyl borates as derivatization procedures is reported. For measurements, several hyphenated approaches based on GC-AAS, MIP-AES, and GC-MIP-AES have been used. A multifaceted analytical approach to identify OMC species, with a focus on Sn, Hg, and Pb stability as a governing factor, is highlighted. It is necessary to assess recovery from CRMs, recovery from the isotope dilution methodology, and the standard addition method to obtain valuable information.