N-nitrosamines are compounds with the general chemical structure R1N(-R2)-N=O that are formed by oxidation reactions of secondary or tertiary amines with the help of a nitrosating agent. Showing mutagenic and carcinogenic effects on various organs and tissues in humans they have become the subject of numerous analytical tests in recent years. Analytical testing is essential to prevent the formation of N-nitrosamines and their removal from water. In this study, seven N-nitrosamines were analysed: N, N-dibutylnitrous amide (NDBA), N, N-diethylnitrous amide (NDEA), N, N-dimethylnitrous amide (NDMA), N, N-dipropylnitrous amide (NDPA), 4-nitrosomorpholine (NMOR), 1-nitrosopiperidine (NPIP) and 1-nitrosopyrrolidine (NPYR). In order to meet the goal of the study in the form of optimization of the sample preparation procedure for the chromatographic analysis of N-nitrosamines, the Box-Behnken design of experiments with three numerical variables at three levels in combination with the response surface methodology (RSM) was applied. Water samples were prepared by solid phase extraction (SPE) using coconut charcoal as a sorbent. After numerical optimization, a sample volume of 300 ml, an eluent volume of 12 ml and a sorbent drying time of 10 min were used as the optimal conditions for solid phase extraction. Two experiments were performed at optimal conditions, one involving the evaporation of the solvent from the sample on a rotary evaporator, and the other the evaporation of the solvent from the sample in a stream of nitrogen. The presence of N-nitrosamines in the obtained extracts in both cases was confirmed by high-performance liquid chromatography with diode array detector (HPLC-DAD) by applying gradient elution at a flow rate of 0,5 ml/min. A successful separation of all seven N-nitrosamines was carried out on the Kinetex C18 chromatographic column using MilliQ water and acetonitrile as mobile phases. By comparing the obtained responses and extraction efficiency values, it is possible to conclude that evaporation in a nitrogen stream is more efficient for NDMA, NDEA, NDPA and NDBA compared to evaporation on a rotary evaporator. From an economic point of view, the optimization of the SPE procedure ensures the saving of reagents and consumables, as well as the time spent by the scientist.