Microstructured optical fibers (MOF) are a promising tool for improving biosensors, optical sensing, biomedical research, and clinical imaging. Approaches to the modification of the inner surface of microstructured optical fibers with a hollow core (MOF-HC) with polymer and photoluminescent materials using layer-by-layer deposition technology was developed. The method allows not only varying the thickness and charge of the layers, but also controllably introduce functional structures into the layers, in particular nanoparticles. The layer-by-layer deposition of polydiallyldimethylammonium chloride (PDDA) cationic polyelectrolyte with an average molecular weight (200 - 350 kDa) and negatively charged fluorescent nanoparticles - cadmium-free quantum dots (QD) of the AgInS2/ZnS structure, luminescent red (625 nm), orange (606 nm), yellow (570 nm) and green (556 nm) was investigated. QDs of the AgInS2/ZnS core/shell structure were obtained by the one-pot aqueous synthesis and selectively separated by successive deposition into fractions according to the size and color of the luminescence. This ensured the similarity of the properties of QDs with different luminescence colors. It was found that with an increase in the number of bilayers PDDA/QD from 1 to 5, the long-wave shift of the HC-MOF transmittance spectrum is: for layers based on red QD - 10 nm, orange QD - 11 nm, yellow 7 nm and green 8 nm relative to the spectrum of the original HC-MOF. When QD is included in the composition of the photoluminescent coating in the HC-MOF, a decrease in the wavelength of the maximum emission of QD is recorded, while the application of a subsequent layer of PDDA leads to its increase. For citation: Kochergin T.P., Ponomaryova T.S., Goryacheva I.Y. Production and properties of a photoluminescent coating based on semiconductor quantum dots in a hollow core of microstructured glass. ChemChemTech [Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol.]. 2023. V. 66. N 2. P. 85-91. DOI: 10.6060/ivkkt.20236602.6615.