Determination of ticlopidine in human plasma by capillary gas chromatography with ion trap detection

A gas chromatographic method for determination of ticlopidine in human plasma using mass spectrometric detection was developed. A Perkin Elmer model 8500 gas chromatograph coupled to an ion trap detector (ITD) in electron impact mode (EI) was used. The gas chromatograph was fitted with a 30 m×0.32 mm i.d., DB-17 capillary column with a film thickness of 0.25 [mu]m. The compounds were isolated from plasma by Extrelut-1 solid-phase extraction using hexane as the solvent of elution. The detection and quantification limits for this method were 0.005 and 0.01 [mu]g/ml, respectively. The calibration curves were linear from 0.01 and 2.5 [mu]g/ml. Recoveries from human plasma spiked at 0.01 and 2.0 [mu]g/ml ranged from 84.4 and 87.3%. The coefficient of variation (CV) was between 5.1 and 6.9%. The results show that the sensitivity, accuracy and precision of the method are adequate for the determination of ticlopidine in human plasma samples. The ITD in SIM mode allows the unequivocal identification of ticlopidine. The suitability of this method was evaluated in the determination of ticlopidine in plasma from healthy volunteers following oral administration of a dose of 500 mg/day.http://www.sciencedirect.com/science/article/B6TGX-48R7F4V-2/1/7f0e17eaa3f9ec2ce371c06ae41c857

Assessment of Pesticide Residues in Honey Samples from Portugal and Spain

Fifty samples of honey collected from local markets of Portugal and Spain during year 2002 were analyzed for 42 organochlorine, carbamate, and organophosphorus pesticide residues. An analytical procedure based on solid-phase extraction with octadecyl sorbent followed by gas chromatography−mass spectrometry (GC−MS), for organochlorines, and by liquid chromatography−atmospheric pressure chemical ionization-mass spectrometry (LC−APCI-MS), for organophosphorus and carbamates, has been developed. Recoveries of spiked samples ranged from 73 to 98%, except for dimethoate (40%), with relative standard deviations from 3 to16% in terms of repeatability, and from 6 to 19% in terms of reproducibility. Limits of quantification were from 0.003 to 0.1 mg kg-1. Most of the pesticides found in honey were organochlorines. Among them, γ-HCH was the most frequently detected in 50% of the samples, followed by HCB in 32% of the samples and the other isomers of HCH (α-HCH and β-HCH) in 28 and 26% of the samples, respectively. Residues of DDT and their metabolites were detected in 20% of the samples. Of the studied carbamates, both methiocarb and carbofuran were detected in 10% of the samples, pirimicarb in 4% and carbaryl in 2%. The only organophosphorus pesticides found were heptenophos in 16%, methidathion in 4%, and parathion methyl in 2% of honey samples. Results indicate that Portuguese honeys were more contaminated than Spanish ones. However, honey consumers of both countries should not be concerned about the amounts of pesticide residues found in honeys available on the market

Uptake, accumulation and metabolization of the antidepressant fluoxetine by Mytilus galloprovincialis

Fluoxetine, a selective serotonin re-uptake inhibitor (SSRI) antidepressant, is among the most prescribed pharmaceutical active substances worldwide. This study aimed to assess its accumulation and metabolization in the mussel Mytillus galloprovincialis, considered an excellent sentinel species for traditional and emerging pollutants. Mussels were collected from Ria Formosa Lagoon, Portugal, and exposed to a nominal concentration of fluoxetine (75 ng L-1) for 15 days. Approximately 1 g of whole mussel soft tissues was extracted with acetonitrile:formic acid, loaded into an Oasis MCX cartridge, and fluoxetine analysed by liquid chromatography with tandem mass spectrometry (LC-MSn). After 3 days of exposure, fluoxetine was accumulated in 70% of the samples, with a mean of 2.53 ng g(-1) dry weight (d.w.) and norfluoxetine was only detected in one sample (10%), at 3.06 ng g(-1) d.w. After 7 days of exposure, the accumulation of fluoxetine and norfluoxetine increased up to 80 and 50% respectively, and their mean accumulated levels in mussel tissues were up to 4.43 and 2.85 ng g(-1) d.w., respectively. By the end of the exposure period (15 days), both compounds were detected in 100% of the samples (mean of 9.31 and 11.65 ng g(-1) d.w., respectively). Statistical analysis revealed significant accumulation differences between the 3rd and 15th day of exposure for fluoxetine, and between the 3rd and 7th against the 15th day of exposure for norfluoxetine. These results suggest that the fluoxetine accumulated in mussel tissues is likely to be metabolised into norfluoxetine with the increase of the time of exposure, giving evidence that at these realistic environmental concentrations, toxic effects of fluoxetine in mussel tissues may occur. (C) 2016 Elsevier Ltd. All rights reserved

Ochratoxin A in Portugal: A Review to Assess Human Exposure

In Portugal, the climate, dietary habits, and food contamination levels present the characteristics for higher population susceptibility to ochratoxin A (OTA), one of the known mycotoxins with the greatest public health and agro-economic importance. In this review, following a brief historical insight on OTA research, a summary of the available data on OTA occurrence in food (cereals, bread, wine, meat) and biological fluids (blood, urine) is made. With this data, an estimation of intake is made to ascertain and update the risk exposure estimation of the Portuguese population, in comparison to previous studies and other populations

Mortality from gastrointestinal congenital anomalies at 264 hospitals in 74 low-income, middle-income, and high-income countries: a multicentre, international, prospective cohort study

Summary Background Congenital anomalies are the fifth leading cause of mortality in children younger than 5 years globally. Many gastrointestinal congenital anomalies are fatal without timely access to neonatal surgical care, but few studies have been done on these conditions in low-income and middle-income countries (LMICs). We compared outcomes of the seven most common gastrointestinal congenital anomalies in low-income, middle-income, and high-income countries globally, and identified factors associated with mortality. Methods We did a multicentre, international prospective cohort study of patients younger than 16 years, presenting to hospital for the first time with oesophageal atresia, congenital diaphragmatic hernia, intestinal atresia, gastroschisis, exomphalos, anorectal malformation, and Hirschsprung’s disease. Recruitment was of consecutive patients for a minimum of 1 month between October, 2018, and April, 2019. We collected data on patient demographics, clinical status, interventions, and outcomes using the REDCap platform. Patients were followed up for 30 days after primary intervention, or 30 days after admission if they did not receive an intervention. The primary outcome was all-cause, in-hospital mortality for all conditions combined and each condition individually, stratified by country income status. We did a complete case analysis. Findings We included 3849 patients with 3975 study conditions (560 with oesophageal atresia, 448 with congenital diaphragmatic hernia, 681 with intestinal atresia, 453 with gastroschisis, 325 with exomphalos, 991 with anorectal malformation, and 517 with Hirschsprung’s disease) from 264 hospitals (89 in high-income countries, 166 in middleincome countries, and nine in low-income countries) in 74 countries. Of the 3849 patients, 2231 (58·0%) were male. Median gestational age at birth was 38 weeks (IQR 36–39) and median bodyweight at presentation was 2·8 kg (2·3–3·3). Mortality among all patients was 37 (39·8%) of 93 in low-income countries, 583 (20·4%) of 2860 in middle-income countries, and 50 (5·6%) of 896 in high-income countries (p<0·0001 between all country income groups). Gastroschisis had the greatest difference in mortality between country income strata (nine [90·0%] of ten in lowincome countries, 97 [31·9%] of 304 in middle-income countries, and two [1·4%] of 139 in high-income countries; p≤0·0001 between all country income groups). Factors significantly associated with higher mortality for all patients combined included country income status (low-income vs high-income countries, risk ratio 2·78 [95% CI 1·88–4·11], p<0·0001; middle-income vs high-income countries, 2·11 [1·59–2·79], p<0·0001), sepsis at presentation (1·20 [1·04–1·40], p=0·016), higher American Society of Anesthesiologists (ASA) score at primary intervention (ASA 4–5 vs ASA 1–2, 1·82 [1·40–2·35], p<0·0001; ASA 3 vs ASA 1–2, 1·58, [1·30–1·92], p<0·0001]), surgical safety checklist not used (1·39 [1·02–1·90], p=0·035), and ventilation or parenteral nutrition unavailable when needed (ventilation 1·96, [1·41–2·71], p=0·0001; parenteral nutrition 1·35, [1·05–1·74], p=0·018). Administration of parenteral nutrition (0·61, [0·47–0·79], p=0·0002) and use of a peripherally inserted central catheter (0·65 [0·50–0·86], p=0·0024) or percutaneous central line (0·69 [0·48–1·00], p=0·049) were associated with lower mortality. Interpretation Unacceptable differences in mortality exist for gastrointestinal congenital anomalies between lowincome, middle-income, and high-income countries. Improving access to quality neonatal surgical care in LMICs will be vital to achieve Sustainable Development Goal 3.2 of ending preventable deaths in neonates and children younger than 5 years by 2030

Loss of Organochlorine Pesticide Residues during the Infusion Processes of Linden (Tilia cordata Mill.)

Losses of residues of α-hexachlorocyclohexane (α-HCH), β-HCH, γ-HCH, hexachlorobenzene (HCB), heptachlor and its epoxide, p,p‘-DDE, p,p‘-DDD, o,p‘-DDT, p,p‘-DDT, α-endosulfan, β-endosulfan, endosulfan sulfate, aldrin, dieldrin, and endrin, when linden is subjected to three infusion processes, were studied. Compounds were quantified by gas−liquid chromatography with electron capture detection. Higher losses are found for heptachlor epoxide (HE) and o,p‘-DDT, in process 1 and for α-HCH, HCB, HE, and aldrin in procedures 2 and 3. Lower losses are obtained for β-HCH in process 2. The best procedure for infusion preparation was procedure 3

Resíduos de pesticidas em alimentos: Desenvolvimento de estratégias analíticas. Coimbra, ed. aut., 1994, 428 p.

A tese apresenta-se estruturada em sete capítulos. Os dois primeiros referem a revisão dos processos de extracção, purificação, determinação e confirmação dos resíduos de pesticidas descritos na bibliografia científica. No primeiro capítulo, a revisão reporta-se aos organofosforados, enquanto no segundo se refere aos organoclorados. O terceiro capítulo foca as interferências e contaminações, de elevada incidência na análise de resíduos de pesticidas, que induzem o analista menos prevenido a interpretações erróneas. No quarto capítulo referem-se aspectos cruciais relacionados com as implicações toxicológicas disponíveis na literatura científica, ligadas aos resíduos de pesticidas, a contribuição dos mesmos veiculada pelos alimentos e, finalmente, a carga de distintos resíduos presentes no leite, no tecido adiposo, na pele e no sangue de populações em distintos pontos do globo. Nos dois capítulos seguintes desenvolve-se a parte experimental distribuída pelo estudo do comportamento cromatográfico dos pesticidas a analisar, pela validação do(s) método(s) e pela avaliação dos teores em resíduos presentes nas amostras: · no quinto capítulo, a exposição versa a avaliação de resíduos de pesticidas organofosforados como o diazinão, o fosfamidão, o malatião, o cis-mevinfos, o paratião, o paratião-metilo e o paraoxon, no leite e de clorpirifos, etião, fenitrotião e metidatião, no tecido muscular e pele de frango; · no sexto capítulo, a explanação incide sobre resíduos de organoclorados, a, b e g - HCH, HCB, aldrina, p,p’DDE, DDD e DDT e o,p’DDT nas mesmas matrizes citadas no capítulo anterior. O último capítulo incide sobre o estado global da presença de resíduos dos dois grupos de pesticidas nos alimentos estudados, com especial incidência sobre a presença de resíduos violativos

Residuos de pesticidas em alimentos: desenvolvimento de estrategias analiticas

Available from Fundacao para a Ciencia e a Tecnologia, Servico de Informacao e Documentacao, Av. D. Carlos I, 126, 1200 Lisboa / FCT - Fundação para o Ciência e a TecnologiaSIGLEPTPortuga