Name: CLEBSON DE JESUS MACRINO
Type: PhD thesis
Publication date: 31/03/2022
Advisor:
Name |
Role |
|---|---|
| ÁLVARO CUNHA NETO | Co-advisor * |
| WANDERSON ROMÃO | Advisor * |
Examining board:
| Name |
Role |
|---|---|
| ÁLVARO CUNHA NETO | Co advisor * |
| ANDRÉA RODRIGUES CHAVES | External Examiner * |
| JOSÉ LUIZ DA COSTA | External Examiner * |
| PAULO ROBERTO FILGUEIRAS | Internal Examiner * |
| VALDEMAR LACERDA JUNIOR | Internal Examiner * |
Pages
Summary: The area of forensic chemistry has been growing and developing more and more as a research line in Brazil, and thus requires increasingly reliable results due to its importance in criminalistics. Thus, the development of new ones that help this area, whether in the ideification and quantification of drugs or in the fight against fraud, become promising. In this context, the present work explored the development of reference materials from drug samples seized by the Civil Police of the State of Espírito Santo (PC- ES), cocaine, crack and ecstasy tablets. Cocaine was isolated by column croamtography, and presented an isolation yield of 50% for the use of the mobile methanol phase 9: 1 ammonium hydroxide with a purity of 98.37%. Benzyoecgonin was synthesized from cocaine alone, with a yield of 91.16% and a purity of 95.40%. Homogeneity studies for benzyoecgonin indicated that the studied lot was homogeneous based on the statistical test of ANOVA by single factor, with a p-value (0.9959) an average value of 976.7212 μg/mL (1.80% standard deviation), with sbb values equal to 22.6 μg/mL and ubb of 1.03%. Short-term stability showed that benzyoecgonin is stable at temperatures of 22, 5 and -8 ºC in the 15, 30 and 30 day periods respectively. At 22 ºC, an average value of 940.8432 μg/mL (4.36% standard deviation) was obtained with usts equal to 1.22%. At 5 ºC the mean value of 895.1915 μg/mL (5.03% standard deviation) was obtained with usts of 0.28%. And at -8 ºC was found the mean value of 942.2749 μg/mL (2.49% standard deviation) and a value of usts equal to 0.26%. At 50 ºC was unstable, due to the degradation that occurred during the storage process for study. From ecstasy tablets, it was possible to isolate MDMA through HPLC and characterized. An isolation yield of 91.34% m/m was obtained with a relative purity of 89.49%. Studies with europium III complexes have also been carried out for application in the fight against fraud. The complexes [Eu(pic)3.(DVL)3], [Eu(pic)3.( EPK)3] and [Eu(pic)3.(OEN)3] were evaluated as new luminescent markers for application as security elements in Brazilian banknotes. Qualitative luminescence tests were performed on r$ 10, 20, 50 and 100 reais banknotes. The complexes were applied on the surface of the banknotes and were exposed to different wavelengths, 254, 312 and 365 nm (Spectral Video Comparator VSC® 6000) and 320 - 400 nm (Lumatec Superlite 400), with the emission of europium red lightIII. The chemical profile of the complexes was identified in the banknotes LDI(±)MS. The complex [Eu(TTA)3(PRD)(H2O)] was studied to be applied as a luminescent sensor to combat 17 adulteration of gasoline as ethanol. The 5D0→7F2 (612 nm) transition was monitored in relation to the variation of the gasoline:ethanol(complex) ratio in the range of 0-100% (v/v). R2 = 0.9815 and a detection limit of 4.94%.
