Cation-exchange solid-phase and liquid-liquid extraction for the determination of khat alkaloids by reversed phase HPLC-DAD

Leaves of khat (Catha edulis) are masticated to elicit their psycho-stimulating properties, resulting from the presence of the phenylpropylamino alkaloids. The determination of these alkaloids is important in pharmacological, phytochemical, forensic and law enforcement environments. In this study, the use of strong cation exchange-solid phase extraction (SCX-SPE) was investigated as an alternative means of sample purification prior to the determination of cathinone, cathine and norephedrine by reversed phase (C18) high performance liquid chromatography (HPLC). Extraction parameters for SCX, including loading capacity and washing solvents, were established. An existing liquid-liquid extraction (LLE) method was improved in terms of recoveries obtained, by using ethyl acetate as extractant. For pure standards of the khat alkaloids, recoveries ranged from 83 to 97%. Preconcentration, using a Genevac evaporator after the addition of acidified water to the sample, restricted analyte losses when compared to concentration under nitrogen. Although comparable recoveries were obtained when preconcentration was achieved in the presence of acidified water by rotary evaporation, this method is not suitable for large sample numbers. Best recoveries, ranging from 94 to 102%, were obtained by SCX from spiked samples. Although the extraction efficiencies of LLE were lower (87-90%), LLE yielded less complex chromatograms, indicating a purer extract. KEY WORDS: Khat alkaloids, Solid phase extraction, Liquid-liquid extraction, HPLC, Genevac Bull. Chem. Soc. Ethiop. 2015, 29(3), 331-339.DOI: http://dx.doi.org/10.4314/bcse.v29i3.

Slurry nebulization ICP-OES for the determination of Cu, Fe, Mg, Mn and Zn

A method that involves analysis of bovine liver by slurry nebulization and ICP-OES has been developed. This method permits rapid and accurate determination of Cu, Fe, Mg, Mn and Zn in bovine liver. Aliquots of freeze-dried and powdered bovine liver sample were dispersed in 2.0 M HNO3 and sonicated to homogenize the resulting slurries. Bovine liver samples were also microwave digested or subjected to aqueous extraction for comparison of analytical results. Concentrations of Cu, Fe, Mg, Mn and Zn in aqueous slurries, the digests, and aqueous extracts were determined by the ICP-OES using external calibration curves. A student’s t-test showed that the results obtained using the slurry method were in good agreement at 95 % confidence level (CL) with those of microwave digestion or aqueous extraction techniques, except for Fe. To check the accuracy and precision of the slurry method, a bovine liver CRM was analyzed and good agreement was achieved with the certified values at 95 % CL. The results demonstrate inefficiency of aqueous extraction technique for complete removal of Fe in bovine liver sample. KEY WORDS: Bovine liver, ICP-OES, Slurry nebulization, Cu, Fe, Mg, Mn, Zn   Bull. Chem. Soc. Ethiop. 2008, 22(3), 313-321.

Determination of selected organochlorine pesticide (OCP) compounds from the Jukskei River catchment area in Gauteng, South Africa

Organochlorine pesticides (OCPs) are continually detected in the environment due to their increasing applications in agriculture and industry. The presence of OCPs in the environment is not desirable since they are well known to have negative impact in humans, animals and birds. Thus, there has been a continual demand to monitor the presence of OCPs within the environment. Liquid-liquid extraction (LLE) and Soxhlet extraction (SE) methods (using dichloromethane as the extracting solvent,) were optimised and evaluated for the determination of these compounds in surface water (unfiltered and filtered) and sediment samples. The crude extracts obtained were subjected to column chromatography for clean-up. Thereafter, 1 μℓ of the cleaned extracts were injected into the GC equipped with ECD.Percentage recoveries obtained for OCPs ranged from 98.90±7.32 (2,4’-DDE) - 124.1±8.23 endosulfan II (ENDO II) % and from 98.99±5.30 (2,4’-DDE) - 121.1±0.38 (4,4’-DDE) % in spiked triply distilled water and sediment samples respectively. The levels of OCPs obtained in unfiltered environmental water samples ranged from 0.631±0.03 (γ-HCH) -1 540±0.19 ng·mℓ-1 (4,4’-DDT) while levels in filtered water samples ranged from 0.895±0.01 (γ-HCH) - 9 089±0.08 ng·mℓ-1 (HEPTA). Levels of analysed OCPs obtained in sediments ranged from 0.266±0.01 (δ-HCH) - 22 914±2.85 ng·gdw-1 (2,4’-DDE). Analytes adsorbed on the sample bottles used for water samples collection gave levels which ranged from 0.01±0.01 - 1.06±0.02 ng·mℓ-1 for OCPs.The levels obtained from the catchment were significantly higher than the water criteria values recommended by USEPA and DWAF for the protection of the aquatic environment. Levels obtained were also higher than those of other studies conducted so far in South African aquatic environments. There is, therefore, a definite pollution of the Jukskei River catchment by the OCPs studied.Keywords: OCPs, surface water, sediments, liquid-liquid extraction, GC-EC

Levels of selected alkylphenol ethoxylates (APEs) in water and sediment samples from the Jukskei River catchment area in Gauteng, South Africa

There has been a continual search to develop sensitive analytical methods for detecting and determining organic compounds such as alkylphenol ethoxylates (APEs) in environmental samples, since they occur at very low concentration levels. Studies conducted so far in some South African waters have offered little or no information on APEs. The presence of these compounds in environmental samples is not desirable and therefore, needs to be monitored. Water and sediment samples were collected from different sites in the Jukskei River catchment area in the 2005 summer and winter seasons. Liquid-liquid extraction (LLE) and Soxhlet extraction (SE) methods (using 1:1 dichloromethane and methanol as extracting solvents) were optimised, evaluated and used to determine APEs of interest in water (unfiltered and filtered) and sediment samples, respectively. Mean percentage recoveries obtained for APEs in spiked double-distilled water were between 83.1±1.0 (OPnEOS3) and 108.1±3.5 (OP) and for sediments the range was between 96.6±0.9 (OPnEOS1) and 117.1±0.6 (OPnEOS3). The concentration levels of APEs studied in unfiltered environmental water samples were in the range of 0.25(0.03) ng/mℓ (NP) to 92.7(1.11) ng/mℓ (OPnEOS3) and 0.31(0.02) ng/mℓ (NP) to 60.1(0.51) ng/mℓ (OPnEOS3) for filtered environmental water samples. Concentration levels obtained in sediments were from 1.94(0.14) ng/gdw to 941(0.50) ng/gdw (OPnEOS3). Analytes adsorbed on the sample bottle gave concentration levels which ranged from 0.02(0.02) ng/mℓ to 0.42(0.02) ng/mℓ for APEs. All the compounds studied were found at levels higher than the European Union (EU) set levels for the protection of the aquatic environment. Keywords: APEs, surface water, sediments, liquid-liquid, soxhlet, GC-FI

Assessment of the concentration of Cr, Mn and Fe in sediment using laser-induced breakdown spectroscopy

In the present study, laser-induced breakdown spectroscopy (LIBS) has been applied for the determination of levels of Cr, Mn and Fe in sediment samples and the results have been compared with that of flame-atomic absorption spectroscopy (F-AAS). Fourteen sediment samples were collected from Tinishu Akaki River (TAR), Addis Ababa, Ethiopia. Pellets of 24 mm in diameter and 3-5 mm in thickness were prepared using a manual hydraulic press under a pressure of 8000 psi by mixing finely ground sediment samples with boric acid. The concentrations of Cr, Mn and Fe were successfully determined by Q-switched Nd:YAG laser at 1064 nm. Quantification of these metals was conducted against certified reference materials of sediments and soils. The LIBS results for the elements varied from 0.060–0.707 mg/g for Cr, 0.895–3.64 mg/g for Mn and 26.9–71.8 mg/g for Fe. The F-AAS results varied from 0.061–1.37 mg/g for Cr, 1.24–4.46 mg/g for Mn and 49.0–83.3 mg/g for Fe. TAR was found to be heavily polluted with Cr. KEY WORDS: Laser-induced breakdown spectroscopy, Chromium, Manganese, Iron, Sediment, Tinishu Akaki River, Ethiopia Bull. Chem. Soc. Ethiop. 2013, 27(1), 1-13.DOI: http://dx.doi.org/10.4314/bcse.v27i1.

Risk factors associated with mortality and interventions in 472 neonates with interrupted aortic arch: A Congenital Heart Surgeons Society study

ObjectiveWe sought to determine the prevalence of outcomes and associated patient and management factors for neonates with interrupted aortic arch.MethodsFrom 1987 to 1997, a total of 472 neonates were enrolled prospectively from 33 institutions. Competing risks methodology was used to determine simultaneous risk and associated incremental risk factors for death, initial and subsequent left ventricular outflow tract procedures, and arch reinterventions.ResultsOverall survival was 59% at 16 years after study entry but improved with successive birth cohort. In general, risk factors for death in each of the competing risks analyses included lower birth weight, younger age at study entry, type B interrupted aortic arch, and major associated cardiac anomalies. Of 453 patients who had interrupted aortic arch repair, after 16 years 33% had died and 28% had undergone an arch reintervention. Reintervention was more likely for those who had truncus arteriosus repair, interrupted aortic arch repair by a method other than direct anastomosis with patch augmentation, and the use of polytetrafluoroethylene as either an interposition graft or a patch. From study entry, competing risks after 16 years showed that 28% had died and 34% had undergone an initial left ventricular outflow tract procedure. Initial left ventricular outflow tract procedure was more likely for those with single ventricle, type B interrupted aortic arch, bicuspid aortic valve, or anomalous right subclavian artery. Among those who had undergone an initial left ventricular outflow tract procedure, after 16 years 37% had died and 28% had undergone a second procedure.ConclusionAnatomic features affect mortality and initial left ventricular outflow tract procedures, whereas characteristics of the arch repair affect arch reintervention

Phono-spectrographic analysis of heart murmur in children

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Self-reflection and academic performance: is there a relationship?

The purposes of the present study were two-fold: first, to evaluate whether reflection journal writing was effective in promoting self-reflection and learning, and whether students become better at self-reflection if they engage continuously in reflection journal writing. To that end, the reflection journals of 690 first-year applied science students at a local polytechnic were studied by means of an automated coding procedures using software. Data was collected twice, once at the beginning and again towards the end of an academic year. Outcomes of the textual content analyses revealed that students reflected on both the process and contents of their learning: critical review of past learning experiences, learning strategies and summaries of what was learned. Correlational analyses showed weak to moderate inter-relationship

Teachers matter for metacognition : facilitating metacognition in the primary school through teacher-pupil interactions

Despite the ubiquity of Structured Thinking Activities (STAs) throughout primary school education in the UK and beyond, little is known about the ways that activities such as learning logs are used to support pupils to think about and manage their own thinking (i.e., engage with metacognition). Here we investigated how pupils engaged with STAs throughout a school year by conducting an in-depth case study of one Scottish primary four classroom, examining factors that facilitated and/or inhibited pupil metacognition. By triangulating data from participant observation, interviews and document analysis, we found that pupils were often un-motivated to engage with STAs, with responses provided during written and oral activities typically revealing superficial references to classroom topics of interest. Whilst factors such as the classroom culture and the timing of activities were found to influence pupil engagement with STAs, observational data indicated that teacher-pupil interactions are essential for eliciting metacognition from pupils (i.e., via discussions that occurred as part of the STAs). Our findings suggest that teachers play a critical role in encouraging elaboration from pupils in relation to descriptions of their own thinking and learning, particularly when pupils’ initial responses are broad or superficial. We discuss the critical importance of teacher talk for metacognition, emphasising the ‘dual role’ that teachers must play when facilitating metacognition within the classroom.PostprintPeer reviewe