Despite the selectivity and sensitivity of modern analytical techniques, there is a crucial need for sample preparation of analytes before their analysis due to their low concentrations in numerous samples with high levels of matrix interferents. Solid-phase extraction (SPE) is a widely used sample preparation technique for the isolation of target analytes from a mobile phase. Obviously, the choice of the sorbent is a key point in SPE procedures and extraction efficiency depends on the particle size and the surface area of the sorbent. In order to their unique properties such as high surface to volume ratio and enhancement the analyte contact surface nano-particles could increase efficiency of the sample pretreatment methods. This book, therefore, introduces a new class of green nano-sorbents for SPE of organic and inorganic anions. Layered double hydroxides (LDHs) are a family of synthetic two-dimensional nano-structured anionic layered materials that have positively charged layers of metal hydroxides. Because of the presence of large interlayer spaces and the signiﬁcant number of exchangeable anions, LDHs have the potential to be good ion-exchangers and adsorbents.