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Gold nanoparticles (GNPs) are commonly synthesized using the Turkevich method, but there are limitations on the maximum concentration of gold nanoparticles that can be achieved using this method (often < 1 mM (=0.34 mg/mL) gold precursor loading). Here, we report an inverse Turkevich method which significantly increases the concentration of gold nanoparticles (up to 5-fold) in the aqueous phase by introducing poly (vinyl alcohol) (PVA) to the synthesis system for stabilization. The aim of this study is to understand the effect of PVA and other synthesis parameters, such as trisodium citrate and tetrachloroauric acid concentration, with the goal of maximizing concentration while maintaining gold nanoparticle morphology, stability, and narrow size distribution. The size distribution of GNPs is investigated for a range of parameters by dynamic light scattering and electron microscopy, and ultraviolet-visible (UV–vis) spectroscopy is also utilized to explore the localized surface plasmon resonance (LSPR). Further, the interaction between GNPs and PVA is investigated by Fourier-transform infrared spectroscopy. In addition to increasing the gold loading by varying synthesis parameters, we also develop a novel anti-solvent precipitation method for the PVA-coated GNPs, which enables continuous condensation and purification of GNPs by forming a gold/PVA nanocomposite.