ABSTRACT
The present work describes the development of a headspace solid-phase microextraction (HS-SPME) followed by gas chromatography - mass spectrometry (GC-MS) method for the qualitative analysis of compounds in seized ecstasy tablets that can be easily implemented in regular laboratories. HS-SPME with a DVB/CAR/PDMS 50/30 µm fiber was used to extract the ecstasy pills' components, including major and minor ones, in a single extraction/chromatographic run. For HS-SPME, the incubation time (0 min to 30 min), the extraction time (10 min to 40 min) and temperature (40 °C to 80 ºC), the buffer volume (3 mL to 8 mL), the buffer pH (6 to 9) and the NaCl concentration (0 mol/L to 6 mol/L) were evaluated using fractional factorial design. Different split ratios and detector voltages were also evaluated. The optimal compromise between sensitivity and peak resolution was found to be incubation and extraction at 65 ºC for 10 min and 25 min, respectively, 3 mL of pH 9 buffer containing 3 mol/L NaCl, using 40.0 mg of the powdered samples in a 15-mL amber glass vial, and an injection with a split ratio of 1:10 at 260 ºC for 10 min. Under optimal conditions, 44 samples from different seizures were analyzed. Seventy-five compounds were tentatively identified by the proposed method, including active substances, medicines, caffeine, safrole derivatives, synthesis intermediates and solvent residues. The number of tentatively identified compounds per sample varied from 8 to 24, with a mean of 15. Important findings in ecstasy samples, such as norcinamolaurin, α-methyl-1,3-benzodioxole-5-propanamide, α-methyl-3,4-methylenedioxyphenylpropionitrile, acetylsalicylic acid, piperonylonitrile, methyl isobutyl ketone, mesitylene, and 4-[3-(dimethylamino)propyl]- 2,6-dimethylphenol, identified with a frequency higher than 10%, are not found in the literature so far. The method precision, based on relative standard deviation of peak areas, ranged from 5% to 15%, depending on the compound. The method was shown to be simple, relatively fast, precise and a powerful tool for the identification of major and minor components in ecstasy tablets in a single analytical cycle, being useful for screening or quantitative purposes, if authentic standards are available.
ABSTRACT
A Odontologia possui amplo campo de atuação, sendo a Odontologia Legal a especialidade exercida junto a serviços oficiais: Instituto Geral de Perícias, Instituto de Criminalística e Instituto Médico Legal. Nessas instituições, o odontolegista pode proceder a exames de corpo delito, necropsias odontolegais, exames de balística, DNA, exames tanatológicos e antropológicos, entre outros. O presente estudo analisou laudos de exames de corpo de delito de lesões que envolveram o complexo maxilomandibular de pessoas que se submeteram à perícia no Instituto Geral de Perícias do Estado de Santa Catarina entre os anos de 2012 e 2014. No período de estudo foram registrados 14310 laudos, sendo 1210 (8,45%) referentes a lesões maxilomandibulares. Destas, 96,2% eram lesões maxilomandibulares e 3,8% lesões em outras regiões, por mordedura humana. Constatou-se que 97,2% dos laudos envolvendo o complexo bucomaxilofacial foram preenchidos por médicos e apenas 2,8% por cirurgiões-dentistas (AU).
Dentistry has a far-reaching field of activity, being the Legal Dentistry the specialty carried out with official services: General Expertise Institute, Institute of Criminalistics and Legal Medical Institute. In these institutions, the forensic dentist can perform examinations of body delicti, dental-legal necropsies, ballistics tests, DNA, thanatological and anthropological examinations, among others. The present study analyzed reports of body lesions that involved the maxillomandibular complex of people who examined at the General Expertise Institute of the State of Santa Catarina between the years of 2012 and 2014. During the period of study 14,310 reports were registered and 1,210 (8.45%) referring to maxillomandibular lesions. Of these, 96.2% were maxillomandibular lesions and 3.8% lesions in other regions, due to human bite. It was found that 97.2% of the reports involving the oral and maxillofacial complex were signed by medical professionals and only 2.8% by dental surgeons (AU).
