A simple and rapid external standard calibration HPLC method for determination of lumefantrine in dried blood spot samples from malaria patients in Botswana.

A simple external calibration liquid chromatography-diode array detector method was developed, validated, and applied for the determination of lumefantrine (Lum) in dried blood spot (DBS) samples collected from malaria patients in Botswana. The samples were validated in accordance with the United States Food and Drug Administration guidelines for bioanalytical methods after sample preparation using solid-liquid extraction. Separation was achieved using an XTerra C18 column (50 × 4.6 mm, 5 µm), and a binary solvent system of acetonitrile and water adjusted to pH 2.3 was used as the mobile phase. The validated method was applied for the determination of Lum in DBS samples collected from malaria patients infected with Plasmodium falciparum in Botswana. The calibration curve was linear between 0.5 and 12 µg/mL with a coefficient of determination (R2 ) of 0.9996. The limit of detection and the lower limit of quantification were 0.5 and 1.4 µg/mL, respectively. The efficiency of extraction measured as percentage recovery ranged between 84.2% and 107.8% at the three quality control (QC) levels, that is, low QC, mid QC, and high QC. In conclusion, data suggest that the method is suitable for the determination of trace Lum in biofluids and can also be used for therapeutic drug monitoring and pharmacokinetic profiling.

A solid-phase microextraction gas chromatography-mass spectrometry technique for urinary metabolomics of human samples infected with schistosomiasis-Case of the Okavango Delta, Botswana.

We present a GC-MS metabolomics workflow for analyzing metabolites in urine samples infected with schistosomiasis. Schistosomiasis, a neglected tropical disease, affects 85% of the global population, with the majority residing in Sub-Saharan Africa. The workflow utilized in this study involved the utilization of the AMDIS freeware, Metab R for pre-processing, and multivariate statistical classification through partial least squares-discriminant analysis (PLS-DA). This classification aimed to categorize volatile metabolites found in urine samples from humans infected with schistosomiasis. All samples were collected from individuals in Botswana. A solid-phase microextraction-fused silica fiber was used to adsorb volatile metabolites from the urine samples and inserted into the GC-MS injection port for data acquisition. The acquired data were then subjected to AMDIS auto-deconvolution, Metab R pre-processing, and statistical evaluation for metabolite mining. A total of 12 metabolites, including 3-chloropropionic acid and heptadecyl ester with an AMDIS match factor of 96% at an approximated amount of 0.35% and cyclohexylamine with an AMDIS match factor of 100% and approximated amount of 0.39%, were identified. PLS-DA was used for the classification of the metabolites. The method showed good sensitivity and specificity as indicated by the receiver operating characteristic measured by the areas under the curves. Results indicated that metabolomics is a useful tool for mining metabolites because of the variance in metabolite composition of infected and non-infected urine samples.

Untargeted GC-MS metabolomics to identify and classify bioactive compounds in Combretum platypetalum subsp. oatesii (Rolfe) Exell (Combretaceae).

INTRODUCTION: Combretum platypetalum is used in traditional African healing practices against different infections. Unfortunately, no scientific knowledge of its phytochemical composition exists, except for the isolation of two compounds from the leaves. Scientific study has been limited to the leaves only, despite the applications of stems and roots in traditional medicine practice and natural product drug discovery programs. OBJECTIVE: Omics was applied to identify and classify different volatile and semivolatile bioactive compounds in the leaf, stem, and root parts of C. platypetalum. The thermal stability of the plant constituents at 60-65°C extraction temperature by Soxhlet and maceration at room temperature on the type, class, and concentration of compounds in the leaf was further investigated. METHOD: A GC-MS untargeted metabolomics approach, automated deconvolution by the Automated Mass Spectral Deconvolution and Identification System (AMDIS) for GC-MS data, preprocessing by Metab R, and multivariate statistical data analysis were employed in this study. RESULTS: A total of 97 phytoconstituents, including 17 bioactive compounds belonging to the terpenoids, flavonoids, long-chain fatty acids, and other unclassified structural arrangements distributed across C. platypetalum, were identified for the first time. A correlation (r = 0.782; P = 0.000) between Soxhlet and maceration extraction methods relative to resolved chromatographic peak areas of metabolites was established. CONCLUSION: Findings corroborate the reported bio-investigation of its leaf extracts, its traditional uses, and previous findings from the Combretum genus. The results substantiate the possible applications of C. platypetalum in natural product drug discovery and provide a guide for future investigations.

Polychlorinated dibenzo-p-dioxin/dibenzofurans (PCDD/Fs) contamination in sediments and fish from Msimbazi River in Dar es Salam, Tanzania: patterns, sources, and their exposure to humans.

Results of a two-dimensional gas chromatograph time of flight mass spectroscopy (GCXGC-TOFMS) determination of polychlorinated dibenzo-p-dioxin (PCDDs) and polychlorinated dibenzofurans (PCDF) in sediments and catfish samples collected from the Msimbazi River are presented here. Samples were extracted using USEPA Method 1613. PCDD/Fs congeners in sediments ranged from 2.0 to 393.0 and 0.7 to 654.8 pg/g in the dry and wet seasons, respectively. 1,2,3,4,7,8,9-HepCDF was detected at the highest concentration, but all were lower than the USA action level of 1000 pg/g. Toxicity for each of the sampling points ranged from 19.7 to 36.5, with a mean concentration of 27.0 pg WHO 2005-TEQ g-1 in the dry season and 2.0 to 38.7 with a mean concentration of 20.7 pg WHO 2005-TEQ g-1 in the wet season. Analysis of variance (ANOVA) showed that there was no significant difference between PCDD/Fs TEQ during the dry and wet seasons (p = 0.08; α = 0.05). The highest TEQ value was estimated at Jangwani in the wet season. Toxicity of PCDD/Fs in catfish collected from the Msimbazi River ranged from 9.3 to 145.2, with a mean of 61.2 pg WHO2005-TEQg-1. Tetrachlorodibenzo dioxin (2, 3, 7, and 8-TCDD) was detected in all fish samples and ranged from 3.5 to 12.7 with a mean of 8.1 pg/g. The concentration of TCDD in fish exceeded the Agency for Toxic Substance and Diseases Registry MRL, thus posing a probable high risk to people whose dietary requirements depend on fish from the Msimbazi River.

Mass spectrometry based metabolomics for small molecule metabolites mining and confirmation as potential biomarkers for schistosomiasis - case of the Okavango Delta communities in Botswana.

INTRODUCTION: Metabolomics for identifying schistosomiasis biomarkers in noninvasive samples at various infection stages is being actively explored. The literature on the traditional detection of schistosomiasis in human specimens is well documented. However, state-of-the-art technologies based on mass spectrometry have simplified the use of biomarkers for diagnostics. This review examines methods currently in use for the metabolomics of small molecules using separation science and mass spectrometry. AREA COVERED: This article highlights the evolution of traditional diagnostic methods for schistosomiasis based on inter alia microscopy, immunology, and polymerase chain reaction. An exhaustive literature search of metabolite mining, focusing on separation science and mass spectrometry, is presented. A comparative analysis of mass spectrometry methods was undertaken, including a projection for the future. EXPERT COMMENTARY: Mass spectrometry metabolomics for schistosomiasis will lead to biomarker discovery for noninvasive human samples. These biomarkers, together with those from other neglected tropical diseases, such as malaria and sleeping sickness, could be incorporated as arrays on a single biosensor chip and inserted into smartphones, in order to improve surveillance, monitoring, and management.

A fast-screening dispersive liquid-liquid microextraction-gas chromatography-mass spectrometry method applied to the determination of efavirenz in human plasma samples.

We demonstrate the suitability of a fast, green, easy-to-perform, and modified sample extraction procedure, i.e., dispersive liquid-liquid microextraction (DLLME) for the determination of efavirenz (EFV) in human plasma. Data acquisition was done by gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode. The simplicity of the method lies in, among others, the avoidance of the use of large organic solvent volumes as mobile phases and non-volatile buffers that tend to block the plumbing in high-performance liquid chromatography (HPLC). Chromatographic and mass spectral parameters were optimized using bovine whole blood for matrix matching due to insufficient human plasma. Method validation was accomplished using the United States Food and Drug Administration (USFDA) 2018 guidelines. The calibration curve was linear with a dynamic range of 0.10-2.0 µg/mL and an R2 value of 0.9998. The within-run accuracy and precision were both less than 20% at the lower limit of quantification (LLOQ) spike level. The LLOQ was 0.027 µg/mL which compared well with some values but was also orders of magnitude better than others reported in the literature. The percent recovery was 91.5% at the LLOQ spike level. The DLLME technique was applied in human plasma samples from patients who were on treatment with EFV. The human plasma samples gave concentrations of EFV ranging between 0.14-1.00 µg/mL with three samples out of seven showing concentrations that fell within or close to the recommended therapeutic range.

Comparison of Soxhlet and reflux techniques for extraction and characterisation of potential endocrine-disrupting compounds from solid waste dumpsite soil.

Landfill leachate contains a myriad of hazardous chemicals; as such, they should always be planned and constructed following approved guidelines. A sample of soil collected from the old quarry designated as the official solid waste disposal site in Maseru, the capital city of Lesotho, was exposed to two extraction techniques, namely Soxhlet and reflux extractions, for characterisation of the potential endocrine-disrupting chemicals in the leachate. Principal component analysis was used to compare the extractability of these chemicals between the two methods, and it revealed that phthalates extract better in Soxhlet than in reflux extraction. Other compounds do not show as much difference. Qualitative analysis of the extracts revealed several compounds of environmental health interest, namely anthracene, bis-di-ethylhexyl-phthalates and di-tert-butylphenol. A review of the literature on some of the annotated compounds was explored for the likely sources thereof. It was discovered that most of the compounds that were identified have plastic origins and are listed as potential endocrine disruptors. The identified compounds were similar to those reported elsewhere in the literature.

Assessment of Heavy-Metal Pollution in Sediments and Tilapia Fish Species in Kafue River of Zambia.

We report results from an evaluation of the levels of heavy metals, i.e., copper (Cu), cadmium (Cd), lead (Pb), nickel (Ni), manganese (Mn), chromium (Cr), and iron (Fe) in sediment and tilapia fish samples from a wide stretch of the Kafue river of Zambia. In sediment samples, the highest Pb and Fe concentrations were recorded at Hippo Dam, i.e., 36.2 ± 0.1 mg/kg dw and 733 ± 37 mg/kg dw at Kafue Town, respectively. Other notably high metal concentrations in sediment were Cr at Kafue Bridge (42.5 ± 0.1 mg/kg dw [dw]), Cu at Mpongwe (233 ± 5 mg/kg dw), and Mn at Kafue Town (133 ± 1 mg/kg dw); it was highest at Ithezi Tezhi Dam at 166 ± 1 mg/kg d. Three fish species, i.e., three-spot bream Tilapia andersonii, red-breasted bream T. rendalli, and nile tilapia Oreochromis niloticus were evaluated for levels of the seven metals. The concentrations of the metals in these fish species afforded estimation of the biota sediment-accumulation factor, which is the ratio of the concentration of the metal in liver to that in the sediment. The coefficients of condition (K) values, which give an indication of the health of the fish, were also estimated. The K values ranged from 2.5 ± 0.5 to 5.1 ± 0.6 in all of the three fish species. Partial least squares analysis showed that heavy metals are generally sequestered evenly in all of the parts of all of the three fish species except for elevated levels of Mn, Cd, and Pb in the liver samples.

GC-MS determination of targeted pesticides in environmental samples from the Kafue Flats of Zambia.

Results of a GC-MS analysis for targeted pesticides i.e. dieldrin, endosulfan, pp-DDT, endrin, HCB, heptachlor, mirex and aldrin in the Kafue Flats of Zambia are presented. Analysis was done in soils, sediments, water and vegetation samples from the Lochinvar and Blue Lagoon National Parks along the Kafue River. A validated analytical method that was used gave recoveries in a spiked soil sample ranging between 60 % and 100 % with limits of detection (LODs) ranging from 0.94 to 8.0 ng/g. The targeted pesticides were not detected in all the samples i.e. were below LODs. Screening using the Automated Mass Spectral Deconvolution and Identification System (AMDIS) simplified the analysis due to its power of deconvolution and identification of analytes of interest.

Pre-electrospray ionisation manifold methylation and post-electrospray ionisation manifold cleavage/ion cluster formation observed during electrospray ionisation of chloramphenicol in solutions of methanol and acetonitrile for liquid chromatography-mass spectrometry employing a commercial quadrupole ion trap mass analyser.

We have observed unusual mass spectra of chloramphenicol (CAP) in solutions of methanol or acetonitrile showing intense ions at m/z 297, m/z 311, m/z 325 and m/z 339. The observed ions were different from those which are traditionally observed in the full scan ESI mass spectra of CAP with ions of m/z 321, m/z 323 and m/z 325. We have evidence to show that this process starts with offline methylation of CAP in solutions of methanol or acetonitrile to give m/z 339. Investigations using nuclear magnetic resonance (NMR) spectroscopy showed that there is a methylene group somewhere within the CAP molecule but not attached to any of the carbon atoms when the CAP is dissolved in methanol or acetonitrile before infusion into the mass spectrometer. The possible locations of attachment were speculated to be the electronegative atoms apart from the chlorine atoms due to valence considerations. The methylene group is attached to the nitrogen atom and forms a bond as observed in the MS/MS spectra of m/z 297, m/z 311, m/z 325 and m/z 339 which give m/z 183 as the base peak in all cases. Further experiments showed that there is cleavage of the methylated CAP molecule followed by cluster ion formation involving addition of methylene groups to the CAP fragment with m/z 183 to produce ions of m/z including m/z 297, m/z 311, m/z 325 and m/z 339. This process occurs in the mass spectrometer in the region housing the tube lens and is triggered when the ions are accelerated through this region by application of a negative tube lens offset voltage. This region affords collision of the charged droplets with a collision gas in this case nitrogen to strip the droplets of their solvent molecules. Experiments to follow the intensities of m/z 183, m/z 311, m/z 321, m/z 323, m/z 325 and m/z 339 as the tube lens offset voltage was varied were done in which the intensities of m/z 311, m/z 325 and m/z 339 were observed to be at their peak when the tube lens offset voltage was set at -40 V. When the tube lens offset voltage is swung to +40 V, thus decelerating the ions through the capillary skimmer region via the tube lens, the traditionally observed spectra with m/z 321, m/z 323 and m/z 325 were observed.

Mapping polychlorinated dibenzo-p-dioxins/dibenzofurans in soils around Pugu municipal dump site in Dar es Salaam, Tanzania: Implications on dermal and soil ingestion exposure for people in the peripheral.

Experimental data on the contribution of a dump site in Tanzania as a point source of the 17 possible congeners of PCDD/Fs to the environment is presented. Dry and wet season samples were collected around Pugu municipal dump site followed by GCxGC-TOFMS analysis. The dominant congeners were OctaCDD, 1,2,3,4,6,7,8-HepCDF; 1,2,3,4,6,7,8-HeptaCDD and 1,2,4,7-PeCDD. The concentrations of the congeners expressed as TEQ WHO2005 ranged from 11.69 to 48.97 pg/g with a mean of 29.44 pg/g for the dry season and TEQ WHO2005 4.13-85.82 pg/g with a mean of 41.51 pg/g for the wet season. These levels were speculated high enough to accumulate in free-range chickens and cause harmful effects to humans that consumed them especially residents around Pugu dump site. Exposure of people to PCDD/Fs through dermal absorption and soil ingestion were estimated using the VLIER-HUMAAN Mathematical model. Exposure through dermal absorption was estimated to be 1.2 × 10-4 and 9.8 × 10-6 ng TEQ/kg day for children and adults respectively while through soil ingestion via consumption of contaminated foods and other sources was 0.0045 and 0.27 ng TEQ/kg day for children and adults respectively. These values however were well below the WHO tolerable daily intake. Generally, there was no significant variation for total PCDD/Fs in the dry and wet season (α = 0.08). Strong positive correlation (r = 0.94) between total PCDD/Fs and organic matter content was observed during the wet season.

Evaluation of endocrine disruptor levels in Kafue Lechwe (Kobus leche kafuensis) samples from the Blue Lagoon National Park of Zambia.

The concentrations of endocrine disruptors were determined in 36 liver tissue, serum and whole blood sample extracts drawn from 15 Blue Lagoon National Park Kafue lechwe. Out of 10 analytes evaluated, 89% of the sample extracts showed very high dieldrin concentrations of between 0.08­100 µg/mL in serum, 0.08­24.8 µg/mL in whole blood and 0.08­4.6 µg/g wet weight in liver tissue extracts. pp-DDE was detected in 83% of the sample extracts at 0.006­5.1 µg/mL in serum, 0.006­8.5 µg/mL in whole blood and 0.006­0.12 µg/g wet weight in liver tissue extracts. There was strong correlation between pp-DDE and dieldrin in all the three matrices. Deltamethrin and endosulfan detected at 50% frequency each. Percent recoveries in spiked laboratory blanks ranged between 60­100% while calculated detection limits ranged from 0.004 to 0.21 µg/mL for all the endocrine disruptors evaluated.

Monitoring polychlorinated dibenzo-p-dioxins/dibenzofurans and dioxin-like polychlorinated biphenyls in Africa since the implementation of the Stockholm Convention-an overview.

Polychlorinated dibenzo-p-dioxin (PCDDs), polychlorinated dibenzofurans (PCDF), and dioxin-like polychlorinated biphenyl (dl-PCB) are groups of toxic compounds released into the environment as unintentional by-products of combustion. They persist, bioaccumulate through the food chain, and cause adverse health effects. This review attempts to collate available information on the release of PCDD/Fs and dl-PCBs and other critical data relevant to their monitoring in Africa during the existence of the Stockholm Convention (SC). Much as the implementation of the SC may be lagging, literature showed that there has been encouraging efforts that have been made with respect to PCDDs/Fs and dl-PCBs monitoring in Africa. Results from a global monitoring study showed that PCDD/Fs released to air in Africa stood at 18-532 fg WHO98 TEQ/M3 while dl-PCBs were 7-278 fg WHO98 TEQ/m3. In human milk, the total concentration of PCDD/Fs, i.e., WHO 2005 TEQ LB has been reported to range from 0.5 ng/g fat to 12 ng/g fat. Fourteen laboratories in Africa participated in inter-laboratory assessments of persistent organic pollutants (POPs) with two specifically for PCDD/Fs analysis. This shows that some efforts are being made to boost capacity in Africa. Levels of PCDDs/Fs and dl-PCBs in clay consumed by pregnant women have been reported in Cameroon, Democratic Republic of Congo (DRC), Nigeria, Zimbabwe, Cote d'Ivoire, and Uganda with a maximum concentration of 103 pg TEQ/g. This finding was very significant since women are the most impacted through exposure to POPs, a fact that is acknowledged by the SC.

Comparison of efficiencies of selected sample extraction techniques for the analysis of selected antiretroviral drugs in human plasma using LC-MS.

INTRODUCTION: Sample preparation in bio analytical chemistry poses a challenge because it can be compound dependent. We compared six sample extraction techniques i.e. QuEChERS (Q), liquid extraction (LE), protein precipitation (PPT), Q-PPT, Q-LE and LE-PPT for the extraction of antiretroviral drugs emtricitabine, tenofovir, efavirenz, lopinavir and rotinavir in human blood plasma. METHOD: A multiple reaction monitoring liquid chromatography- tandem mass spectrometry method for the determination of the same antiretroviral drugs developed and validated in this laboratory was used. Comparisons were based on the efficiencies of extraction, the precisions and accuracies. Using United States Food and Drug Administration guidelines, analytical performance characteristics i.e. limits of detection, lower limits of quantification and upper limits of quantification were also compared. RESULTS: The percent mean recoveries ranged between 68.8 and 81.2% for single modes and 52.4-70.5% for mixed mode techniques. The precisions of all the extraction techniques were within the Using United States Food and Drug Administration guidelines acceptable range of <15% at all concentration levels for all analytes. Accuracy ranged between 8.73 and 65.94% for single mode techniques and between 21.73 and 51.59% for mixed mode techniques. DISCUSSION: The mixed modes gave slightly lower recoveries but Q-LE compared well with the single modes at slightly higher spike levels. Limits of detection for all the six sample preparation techniques fell below the clinically relevant therapeutic range of approximately 3-8ppm. Therefore all techniques can be employed for routine therapeutic drug monitoring studies.

Determination of endocrine disruptors in Kafue lechwe (Kobus leche kafuensis) samples from the Lochinvar National Park of Zambia.

Analysis of serum, whole blood and liver tissue samples from Kafue lechwe in the Lochinvar National Park of Zambia for suspected endocrine disrupting compounds revealed high concentrations for some of the compounds. 45 samples of serum, whole blood and liver tissue were extracted by liquid-liquid extraction followed by an analysis using Gas Chromatography-Electron Capture Detection (GC-ECD). The following endocrine disruptors were analyzed: deltamethrin, aldrin, endosulfan, dieldrin, pp-DDD, heptachlor, d-t-allethrin, pp-DDE, endrin and pp-DDT. For all the samples, dieldrin showed the highest concentration ranging from 1.7 to 44.4 microg/ml in serum and whole blood sample extracts and 0.10-5.1 microg/g wet weight in liver sample extracts. The most frequently detected was deltamethrin in 62% of the samples. Percent recoveries in spiked laboratory blanks ranged between 60% and 100% while calculated detection limits ranged from 0.004 to 0.21 microg/ml for all the endocrine disruptors evaluated. Where endocrine disruptors were detected, the concentrations of most of them far exceeded the maximum residue limits (MRLs) and the extraneous maximum residue limits (EMRLs) set by the Codex Alimentarius of the United Nations (UN), Food and Agricultural Organization (FAO).

Analysis of the level of comprehension of chemical hazard labels: a case for Zambia.

We have surveyed the impact of chemical hazard label elements on four target sectors, i.e. the agricultural, industrial, transport and the consumer (the general public) sectors, in order to assess the type of reactions the respondents perceive to a given chemical label element such as symbol, hazard phrase, color, and hazard signal word. The survey revealed that the level of education, gender and/or age did not influence the respondents' perception of the extent of hazard but rather familiarity or frequency of use of the chemicals and acquaintance with chemical label elements was significant in the assessment of the extent of perceived hazard posed by a given chemical. Symbols such as the St Andrews Cross--though common--is virtually not understood by more than 80% of the respondents in all the sectors. We noted that respondents appreciate symbols they can relate to, which are flame-like, ghost-like and exert immediate impacts to respondents. Color codes have found use in the agriculture sector because of their ease to be recalled especially by the majority of illiterate farm workers. The survey revealed that red in agricultural circles is well associated with high toxicity while other colors such as yellow and blue can not clearly be associated with hazard. The word "toxic" is not used in the industry and transport sectors where the most hazard signal word is "danger". The Globally Harmonized System (GHS) classification adopted "danger" and "warning" for use as signal words. The survey revealed that effective chemical hazard symbols must not be too abstract to the client but should contain features that are known or easily comprehended.

Distribution of copper, lead, cadmium and zinc concentrations in soils around Kabwe town in Zambia.

The extent of pollution of the environment as a result of mining activities in Kabwe, the provincial capital of Central province in Zambia has not yet been evaluated. Mining of lead and zinc were the core activities of Kabwe mine while cadmium and silver were produced as by-products. The smelting processes produced a significant amount of copper. The spatial distribution of four heavy metals in soils in the northern, eastern, southern and western directions of the mine was analyzed using atomic absorption spectrometry (AAS). Samples were collected up to 20 km in each direction from the mine. Results were consistent with the wind flow patterns in the town. Results ranged between 0.08 and 28 mg kg(-1) (Cd); 0.20 and 0.61 mg kg(-1) (Cu); 0.10 and 758 mg kg(-1) (Pb) and 0.40 and 234 mg kg(-1) (Zn) suggesting high precipitation of metals from the core mining activities. These concentrations were for only the fractions of metals extractable by 0.5M nitric acid and that could be available for plant uptake in the environment. The distribution of metals indicated a decrease of metal concentrations with distance from the mine, which confirmed that precipitation due to mining activities was the main cause of soil contamination.

An Investigation of Liquid Chromatography-Mass Spectral Attributes and Analytical Performance Characteristics of Tenofovir, Emtricitabine and Efavirenz in Human Plasma.

Liquid chromatography (LC) and mass spectral behavior and analytical performance characteristics of efavirenz (EFV), emtricitabine (EMT) and tenofovir (TFV), i.e., individual components of Atripla(®), were probed. This was followed by estimation of their analytical performance characteristics employing LC and a parallel direct infusion sample introduction procedure. Performance characteristics using both types of sample introduction procedures were compared. Using liquid chromatography-mass spectrometry (LC-MS), linearities, i.e., correlation coefficients of the calibration curves of EFV, EMT and TFV, ranged between 0.9300 and 0.9990 in the full scan, selected ion monitoring and mass spectrometry/mass spectrometry (MS-MS) modes. The limits of detection (LODs) ranged between 0.5 and 11.6 µg/L. The lower limits of quantification (LLOQs) and the upper limits of quantification (ULOQs) were in the ranges of 0.9-23.2 and 1.6-38.7 µg/L, respectively. The LODs ranged between 0.8 and 114.7 µg/L. The LLOQs and the ULOQs were in the ranges of 1.6-29.4 and 2.7-49.0 µg/L, respectively. In the case of EMT, sodiated molecular ion at m/z 270 was used to adduce analytical performance characteristics from which lower detection limits were obtained compared with those in the literature where [M+H](+) at m/z 248 was used.

Linking environmental exposure with public health: dichlorodiphenyltrichloroethane extracted from soils and water of recently exposed communities of selected locations in Zambia.

BACKGROUND: In 2000, a Zambian private mining company reintroduced the use of dichlorodiphenyltrichloroethane (DDT) to control malaria in two districts. From 2000 to 2010, DDT had been applied in homes without any studies conducted to ascertain its fate in the environment. We aimed to quantify the presence of DDT and its metabolites in the soil and water around communities where it was recently used. METHODS: We collected superficial soil and water samples from drinking sources of three study areas. DDT was extracted by QuEChERS method and solid phase extraction for soils and water, respectively. Analysis was by gas chromatography-mass spectrometry. A revalidated method with limits of detection ranging from 0.034 to 0.04 ppb was used. RESULTS: Median levels of total DDT were found at 100.4 (IQR 90.9-110) and 725.4 ng/L (IQR 540-774.5) for soils and water, respectively. No DDT above detection limits was detected in the reference area. These results are clinically significant given the persistent characteristics of DDT. CONCLUSION: DDT presence in these media suggests possible limitations in the environmental safeguards during IRS. Such occurrence could have potential effects on humans, especially children; hence, there is a need to further examine possible associations between this exposure and humans.

Comparative chromatography-mass spectrometry studies on the antiretroviral drug nevirapine-analytical performance characteristics in human plasma determination.

A contrast between the analytical performance characteristics using gas chromatography-mass spectrometry (GC-MS) liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-ultraviolet (LC-UV) detection for the determination of the antiretroviral drug (ARV) nevirapine (NVP) in fortified human plasma after QuEChERS extraction has been made. Analytical performance characteristics, i.e. linearities, instrument detection limits (IDLs), limits of quantitation (LOQs), method detection limits (MDLs), % mean recoveries and the corresponding relative standard deviations (%RSDs) were estimated using techniques above. Using GC-MS, the correlation coefficients (r(2)) were ≥0.990, which were deemed acceptable linearities. The MDLs ranged between 11.1-29.8µg/L and 13.7-36.0µg/L using helium and hydrogen carrier gases respectively. The LOQs ranged between 16.5-66.7µg/L and 28.4-98.7µg/L using helium and hydrogen carrier gases respectively with a % mean recovery of 83% and %RSD of 4.6%. Using LC-MS and LC-UV, the correlation coefficients (r(2)) were ≥0.990. The MDLs were ranged between 3.14 and 47.1µg/L. The LOQs ranged between 2.85 and 90.0µg/L respectively. The MDLs using GC-MS, LC-MS and LC-UV were below the therapeutic range for NVP in human plasma is considered to be between 2300µg/L (Cmin) and 8000µg/L (Cmax). This study also demonstrated that helium can be substituted with hydrogen which is relatively cheaper and easily obtainable even by use of a generator.