Sertindole is an "non-typical" neuroleptic extensively used for the treatment of schizophrenic patients. The detection of intoxication with this medication implies the necessity of development of the optimal methods for its isolation from the biological materials and further identification. The objective of the present work was to study the influence of various factors on the efficiency of sertindole extraction from solutions, the elaboration of the methods for its isolation from biological objects, detection, and quantitative determination in the extracts from these objects. Investigations into the influence of various factors on the isolation of sertindole from solutions included characteristic of the chemical nature of the organic solvent and the electrolyte, measurements of pH, time and frequency of extraction with the use of UV spectrophotometry. Isolation of sertindole from the liver, kidneys, brain, heart, gastric and intestinal contents was carried out by the method of A.A. Vasil'ev. Moreover, we have developed an original method for the detection of sertindole in the extracts using TLC, UV spectrophotometry, and HPLC. The qualitative determination of sertindole in the extracts from the internal organs, blood plasma, and urine was performed by HPLC. The optimal conditions for sertindole liberation from the extracts have been found and TLC-screening conditions proposed. The TLC, UV spectrophotometric, and HPLC techniques specially modified for the determination of sertindole in the extracts were used. It was shown that the maximum amounts of sertindole were present in the liver and brain within 24 hours after acute poisoning. In the kidneys, stomach, and intestines, it accumulated in smaller quantities Extracts from the heart did not contain sertindole. Maximum efficiency of the sertindole extraction during 24 hours was achived from blood plasma.