[en] A qualitative and quantitative analytical technique of low-molecular components of chemical and radiation-chemical decomposition of 2-deoxy-2-[¹⁸F]fluoro-D-glucose, 2-[¹⁸F]FDG radiopharmaceutical was developed for its extended quality control by HPLC with mass-spectrometric electro-spray ionisation detector (ESI MS). The analysis constituted from the liquid chromatography on silica gel NH₂ bonded column combined with mass-spectrometric, UV-VIS, refraction index and radiometric detectors. A modern LC/MS system (Agilent 1100) was demonstrated to be suitable not only for identification of unknown analytes, but also for complex analysis of solutes except [¹⁸F]F^-. This was advantageous for the 2-[¹⁸F]FDG autoradiolysis assessment about which no data were published. For comparative purposes, were used a classic thin layer chromatography (TLC) on silica gel with mobile phase acetonitril: water at 95:5 v/v, and HPTLC on NH₂ modified silica gel like the LC column. Mobile phase was identical as by LC/MS method (acetonitril: 4 mM aqueous solution of ammonium formate 80:20 v/v). Retention times of reference samples: fluorodeoxyglucose, glucose, mannose, arabinose, deoxyglucose, gluconic and glucuronic acids at HPLC were established. Optimal performance of the ESI MS detector was discovered in negative ions mode or single ion monitoring (SIM) regime. The most intensive signal was observed for all analyte molecules association with formate anion HCOO^- and also for negative ions of deprotonised molecules. All acids appeared in the form of their lactones. FDG and Glc exhibited tendency for formation of a mixed associate charged by HCOO^- anion. On the amine bond silica gel HPTLC column, FDG is poorly separated from fluoride, which even in presence of Kryptofix 2.2.2 remains on the start like on the silica gel layer. At LC-MS Kryptofix provides a very well measurable signals of associates with NH⁴⁺ a H⁺ ions in positive mode of ESI MS. Concentration of (¹⁹F)FDG carrier in 2-[¹⁸F]FDG preparation was found to be 6 mg · dm^-3 and in combination with a radiometric detector the specific activity 6.6 GBq · μmol^-1 of 2-[¹⁸F]FDG was found. The main oxidation products of (¹⁹F)FDG and glucose by Fenton's reagent were arabonic acid at 14-23% yield, gluconic acid 12%, both glucuronic acid and arabinose at 5%. In case of (¹⁹F)FDG among the principal products 2-fluorgluconic acid and 2-fluorgluconic acids by 2.7 % and 4% yields respectively were identified. The dose rates in real solutions of 2-[¹⁸F]FDG, as well as the radiation-chemical yields of radioactive (fluorinated), but also further products of autoradiolysis of 2-[¹⁸F]FDG radiopharmaceutical were assessed. Dose rate comprises about 140 Gy · h^-1, the annihilation radiation contribution being about 50% of the dose. As the main autoradiolysis products of 3.3 · 10^-5 M solution of 2-[¹⁸F]FDG were established: glucose (as additive) - 0.14 mM, arabinose - 2.8 μM (G=0.07/100 eV), gluconic (G=0.05 /100 eV) and glucuronic acids (1.8 - 0.5) μM (G=0.01/100 eV). All 2-[¹⁹F]fluorogluconic, 2-[¹⁹F]fluorogluconic, arabinose and araburonic acids occurred under 0.5 μM concentration. The LC/MS system combined with a radiometric detector discovered two radioactive products of autoradiolysis of 2-[¹⁸F]FDG: 2-[¹⁸F]fluorogluconic and 2-[¹⁸F]fluoroglucuronic acids, which were established by quantitative calibration. The radiation-chemical yield of glucuronic acid is G=0.004 /100 eV and 2-gluconic acid is about 0.003/100 eV. 2-(¹⁸F)fluoroglucuronic acid occurrence was about (0.51 ± 0.10 ) % of 2-(¹⁸F)FDG activity, and 2-(¹⁸F)fluorogluconic acid (0.30 ± 0.04) %. Activity belonging to free (¹⁸F)F- was about (0.20 ± 0.05) %. Radiochemical purity of 2-[¹⁸F]FDG radiopharmaceutical after expiration time was established as (99.0 ± 0.2) % what is much higher than that prescribed by pharmacopoeia (> 95 % 2-[¹⁸F]FDG). The 1% of radiochemical impurities belonging to free [¹⁸F]fluoride and autoradiolysis products should not influence the tomographic imaging. This thesis is the first attempt of a complex quantification of chemical and radiation-chemical stability of physiological solutions of 2-[¹⁸F]FDG. It appeared that the 2-[¹⁸F]FDG is the radiopharmaceutical of high radiation and chemical stability. The thesis also illustrates possibilities of LC/MS/RAD system not only in routine quality control of radiopharmaceuticals but also in research of the new ones