Headspace solid-phase microextraction - gas chromatography - mass spectrometry qualitative screening method for active compounds, adulterants and impurities in ecstasy tablets seized in Northern Santa Catarina State, Brazil.

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.

Biomarkers in Non-Complicated Pregnancy: Insights About Serum Myeloperoxidase and Ultrasensitive C-Reactive Protein.

INTRODUCTION: Pregnancy is characterized by increased innate immune response, with low-grade systemic inflammation. The specific role of MPO during normal pregnancy remains not well understood. Therefore, the aim of this study was to evaluate plasma levels of MPO, hs-CRP, total leukocyte, absolute neutrophil and monocyte counts, in all trimesters of normal human pregnancy compared with non-pregnant controls. In addition, possible fluctuations of MPO according to different inflammatory conditions in the normal gestation were studied. MATERIALS AND METHODS: Case-control study (n=84) developed with 63 normal pregnant women and 21 healthy non-pregnant women. Total leukocyte, absolute neutrophils and absolute monocytes count, hs-CRP and MPO were measured in non-pregnant women and normal human pregnancy. They were evaluated according to the 3 trimesters of pregnancy and systemic low grade inflammatory status, which was identified through increased hs-CRP levels. RESULTS: MPO levels in the normal pregnant women were not elevated in every 3 trimesters of pregnancy (P=0.456) or in systemic inflammation (P=0.446). The hs-CRP levels, total leukocyte, absolute neutrophil and monocyte counts are present in higher concentrations in normal pregnant women in relation to non-pregnant women. CONCLUSIONS: The MPO did not show fluctuations in plasma levels during the 3 trimesters of gestation or in relation to different inflammation conditions. Considering MPO and hs-CRP levels are changed in high cardiovascular risk conditions and MPO levels (unlike hs-CRP) didn't increase during non complicated pregnancy, MPO could be a better biomarker than hs-CRP to monitor these patients.

Changes of metabolic and inflammatory markers in HIV infection: glucose, lipids, serum Hs-CRP and myeloperoxidase.

OBJECTIVE: HIV infection is exacerbated through additional pro-atherogenic mechanisms related to the processes of immune activation, inflammation, coagulation, and the modification of lipoproteins (e.g., particles of high density lipoprotein), contributing to increased cardiovascular risk. The aim of this study was to analyze the serum concentrations of myeloperoxidase (MPO) and other laboratory parameters in HIV-infected patients treated or not with antiretroviral drugs compared to non-infected individuals. MATERIALS/METHODS: The study included 154 volunteers: 47 non-infected individuals (control group - CON), 27 infected and untreated individuals (NTARV group) and 80 treated individuals (TARV group). We analyzed the counts of CD4+ lymphocytes and the viral load of the infected patients, along with the blood count, fasting glucose, total serum cholesterol (CHOL), HDL cholesterol, LDL cholesterol, triglycerides, MPO and high-sensitivity C-reactive protein (CRP) of all study participants. RESULTS: There were significant increases in glucose, CHOL, LDL cholesterol, and triglycerides in the TARV group and significant reductions in the levels of HDL cholesterol for the TARV and NTARV groups. Significantly elevated levels of Hs-CRP were observed only in the TARV group, while levels of MPO were significantly higher in the TARV and NTARV groups compared to the control group. A correlation of MPO with Hs-CRP (r=0.21, p=0.032) was observed for HIV-infected patients, but MPO did not correlate significantly with the other analyzed parameters. CONCLUSIONS: The investigation of early biomarkers for cardiovascular risk evaluation, such as MPO, contributes to the clinical monitoring of HIV-infected individuals. The serum levels of MPO correlated with Hs-CRP and were high in HIV-infected individuals, indicating a possible predictor of cardiovascular events in these patients.

Alterações metabólicas e inflamatórias em condições de estresse oxidativo / Metabolic and inflammatory changes in oxidativestress situations

O estresse oxidativo pode ser definido com o desequilíbrio entre os níveis de compostos pró-oxidantes e antioxidantes, com predomínio dos primeiros. O estado pró-oxidante vem sendo relacionado a várias patologias, como doença cardiovascular, doenças neurodegenerativas, doenças auto-imunes e cânceres, ora como sua causa, em alguns casos como consequência. Assim, torna-se importante determinar quais alterações metabólicas e inflamatórias estão relacionadas com o estresse oxidativo, para auxiliar no diagnóstico e prognóstico dessas doenças. Além dos fatores de risco clássicos, esta revisão chama a atenção para possíveis novos biomarcadores relacionados ao estresse oxidativo, entre estes estão a mieloperoxidase, paraoxonase, homocisteína e determinação do estado antioxidante.

Oxidative stress can be defined as an imbalance between the levels of pro-oxidant and antioxidant compounds, with the former predominating. The pro-oxidant status has been linked to several diseases, such as cardiovascular, neurodegenerative and autoimmune diseases and cancers, at times as the cause, at others as a result. Thus, it is highly relevant to determine which metabolic and inflammatory disorders are associated with oxidative stress, to help in the diagnosis and prognosis of these diseases. In addition to the classical risk factors, this review highlights possible new biomarkers related to oxidative stress, among which are myeloperoxidase, paraoxonase, homocysteine and determination of the antioxidant status.