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We discuss methodology and recent advances in laser-induced SCF synthesis of metal nanoparticles (NPs) and present the results on diagnostics of silver NPs in the pores of several nanoporous transparent matrices: aerogel, nanoporous glass, and oligo(urethane methacrylate). Within the developed approach, a porous sample is impregnated by a silver precursor dissolved in supercritical carbon dioxide or ethanol. Conversion of the precursor into the NPs is stimulated by laser irradiation of the samples under supercritical conditions or at ambient atmosphere after depressurization. The extinction spectra of the composites are measured during the synthesis process, thus the dynamics is observed in real-time. The size and shape of the NPs are estimated by fitting the spectral line shape, providing fast “in-situ” diagnostics. The results of the estimation show a good qualitative agreement with the data obtained by transmission electron microscopy. This work was performed with financial support of RSCF (grant No. 14-33-00017) and RFBR (grant No. 16-02-01022-а).