A supramolecular solvent based liquid–liquid microextraction (SsLLME) system for gold was developed prior to its determination by a microsample injection system coupled with flame atomic absorption spectrometric (MS-FAAS). 1,3,4-Thiadiazole-2,5-dithiol was used as a complexing agent to obtain a hydrophobic complex. The analytical factors affecting the microextraction efficiency, such as the pH, type and volume of supramolecular solvent, amount of complexing agent, ultrasonication and centrifuge time, and sample volume, were investigated. The limit of detection (LOD), enhancement factor (EF) and relative standard deviation (RSD) of the method were 1.5 μg l−1, 51 and 4.2%, respectively. The accuracy of the method was checked by the analysis of CDN-GS-3D Gold Ore certified reference material and addition-recovery tests. The method was successfully applied for the determination of gold in environmental samples.
