Organic micropollutants (MPs) occur ubiquitously in the aquatic environment at trace concentrations, which presents great challenges for environmental monitoring. Solid-phase extraction (SPE) is a widely-used sample preparation procedure that concentrates MPs in environmentally derived water samples. SPE relies on columns packed with an adsorbent material that captures MPs from water samples. Loaded SPE adsorbents can then be eluted with organic solvents to release the captured MPs. The conventional adsorbent used for SPE is a hydrophilic-lipophilic balanced material available from a variety of commercial vendors, often referred to as HLB. These HLB adsorbents feature stability at extreme pHs and high retention of polar and apolar organic MPs. The primary disadvantage of HLB adsorbent materials is price, which often makes sample preparation the most expensive step in an environmental monitoring workflow. In this research, novel porous β-cyclodextrin polymers (P-CDP) were evaluated as an alternative SPE adsorbent. Cyclodextrins are sustainably produced macrocycles of glucose, featuring a hydrophobic interior cavity that forms host-guest complexes with thousands of organic molecules. P-CDP is a polymer of cyclodextrin and is synthesized in one-step, making it relatively inexpensive to produce. The objective of this research was to develop an SPE procedure using P-CDP and compare its performance to a conventional SPE procedure using HLB. A set of 189 MPs were included in the study and the P-CDP method was optimized to maximize efficiency in MP capture and MP release. The optimized P-CDP method exhibits moderate absolute recovery (≥60%) for 135 (75%) MPs and high absolute recovery (≥80%) for 121 (67%) MPs. The conventional HLB method exhibits moderate absolute recovery for 130 (72%) MPs and high absolute recovery for 109 (61%) MPs. The results of this research demonstrate that P-CDP could be used as a cost-effective SPE adsorbent.