An extremely sensitive and simple gas chromatography with mass spectrometry method was developed and completely validated for the analysis of five process-related impurities, viz., 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, 4-hydroxyphenylacetic acid, methyl-4-hydroxyphenylacetate, and 2-[4-{(2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy}phenyl]acetonitrile, in atenolol. The separation of impurities was accomplished on a BPX-5 column with dimensions of 50 m × 0.25 mm i.d. and 0.25 μm film thickness. The method validation was performed following International Conference on Harmonisation guidelines in which the method was capable to quantitate 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid at 0.3 ppm, and methyl-4-hydroxyphenylacetate and 2-[4-{(2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy}phenyl]acetonitrile at 0.35 ppm with respect to 10 mg/mL of atenolol. The method was linear over the concentration range of 0.3-10 ppm for 4-hydroxy-l-phenylglycine, 4-hydroxyphenylacetonitrile, and 4-hydroxyphenylacetic acid, and 0.35-10 ppm for methyl-4-hydroxyphenylacetate and 2-[4-{(2RS)-2-hydroxy-3-[(1-methylethyl)amino]propoxy}phenyl]acetonitrile. The correlation coefficient in each case was found ≥0.998. The repeatability and recovery values were acceptable, and found between 89.38% and 105.60% for all five impurities under optimized operating conditions. The method developed here is simple, selective, and sensitive with apparently better resolution than the reported methods. Hence, the method is a straightforward and good quality control tool for the quantitation of selected impurities at trace concentrations in atenolol.
This paper aims to select the most appropriate rain-based meteorological drought index for detecting drought characteristics and identifying tropical drought events in the Johor River Basin (JRB). Based on a multi-step approach, the study evaluated seven drought indices, including the Rainfall Anomaly Index (RAI), Standardized Precipitation Index (SPI), China-Z Index (CZI), Modified China-Z Index (MCZI), Percent of Normal (PN), Deciles Index (DI), and Z-Score Index (ZSI), based on the CHIRPS rainfall gridded-based datasets from 1981 to 2020. Results showed that CZI, MCZI, SPI, and ZSI outperformed the other indices based on their correlation and linearity (R2 = 0.96-0.99) along with their ranking based on the Compromise Programming Index (CPI). The historical drought evaluation revealed that MCZI, SPI, and ZSI performed similarly in detecting drought events, but SPI was more effective in detecting spatial coverage and the occurrence of 'very dry' and 'extremely dry' drought events. Based on SPI, the study found that the downstream area, north-easternmost area, and eastern boundary of the basin were more prone to higher frequency and longer duration droughts. Furthermore, the study found that prolonged droughts are characterized by episodic drought events, which occur with one to three months of 'relief period' before another drought event occurs. The study revealed that most drought events that coincide with El Niño, positive Indian Ocean Dipole (IOD), and negative Madden-Julian Oscillation (MJO) events, or a combination of these events, may worsen drought conditions. The application of CHIRPS datasets enables better spatiotemporal mapping and prediction of drought for JRB, and the output is pertinent for improving water management strategies and adaptation measures. Understanding spatiotemporal drought conditions is crucial to ensuring sustainable development and policies through better regulation of human activities. The framework of this research can be applied to other river basins in Malaysia and other parts of Southeast Asia.
The most recent set of General Circulation Models (GCMs) derived from the Coupled Model Intercomparison Project Phase 6 (CMIP6) was used in this work to analyse the spatiotemporal patterns of future rainfall distribution across the Johor River Basin (JRB) in Malaysia. A group of 23 GCMs were chosen for comparative assessment in simulating basin-scale rainfall based on daily rainfall from the historical period of the Climate Hazards Group InfraRed Precipitation with Station Data (CHIRPS). The methodological novelty of this study lies in the application of relative importance metrics (RIM) to rank and select historical GCM simulations for reproducing rainfall at 109 CHIRPS grid points within the JRB. In order to choose the top GCMs, the rankings given by RIM were aggregated using the compromise programming index (CPI) and Jenks optimised classification (JOC). It was found that ACCESS-ESM1-5 and CMCC-ESM2 were ranked the highest in most of the grid. The final GCM was then bias-corrected using the linear scaling method before being ensemble based on the Bayesian model averaging (BMA) technique. The spatiotemporal assessment of the ensemble model for the different months over the near-future period 2021-2060 and far-future period 2061-2100 was compared with those under Shared Socioeconomic Pathways (SSPs), namely, SSP1-2.6, SSP2-4.5, SSP3-7.0, and SSP5-8.5. Heterogeneous changes in rainfall were projected across the JRB, with both increasing and decreasing trends. In the near-future and far-future scenarios, higher rainfall was projected for December, indicating an elevated risk of flooding during the end of the North East monsoon (NEM). Conversely, August showed a decreasing trend in rainfall, implying an increasing risk of severe drought. The findings of this study provide valuable insights for effective water resource management and climate change adaptation in the region.
Pristine tropical river systems are coming under increasing pressure from the development of economic resources such as forestry and mining for valuable elements. The Lebir catchment, north eastern Malaysia, is now under development as a result of unregulated tree felling and mining for essential and rare metals. Two sediment cores, one in the upstream reaches and the other from the downstream reaches, were taken from flood prone area of the Lebir River, Malaysia, and analysed for their elemental composition by XRF, specifically Al, Si, Fe, Ca, K, Mg, Mn, V, Cu, Ni, Pb, Cr, Zn, As, Th and U. Activities of fallout radionuclides, 137Cs and 210Pb were also determined to from a geochronological context. The elemental concentrations in the soils were assessed in terms of their enrichment factor and Si, Ca, K, Mg, Mn, V, Cu, Ni and Zn were found not to be enriched, whereas As, Th and U had elevated enrichment factors. The Th and U were particularly enriched in the downstream core indicating inputs from a tributary that drains a catchment with known deposits of Th and possibly U. The results suggest that the growth in economic development is fostering the transport of contaminants by the major rivers which, in turn, is contaminating the riverine floodplains. This points to the need for a more integrated and holistic approach to river basin management to maintain the environmental quality of these fragile aquatic systems.
A newly developed electrochemical sensor for chlorothalonil based on nylon 6,6 film deposited onto screen printed electrode (SPE) with electrochemical modulation of pH at the electrode/solution interface was studied for the first time. Differential pulse cathodic stripping voltammetry (DPCSV) was used to carry out the electrochemical and analytical studies. Experimental parameters such as accumulation potential, initial potential, accumulation time and pH of Britton-Robinson buffer have been optimized. Chlorothalonil gave optimum analytical signal in a medium of 0.04 M Britton-Robinson buffer at pH 6.0. A well-defined reduction peak was observed, at Ep= -0.851 and -0.938 V vs. Ag/AgCl (3.0 M KCl) for both bare SPE and modified SPE, respectively. The peak currents of modified SPE were significantly increased as compared to bare SPE. At the modified SPE, a linear relationship between the peak current and chlorothalonil concentration was obtained in the range from 0.1 to 2.8 × 10-6 M with a detection limit of 1.53 × 10-8 M (S/N= 3). The practical applicability of the newly developed method has been demonstrated on analyses of real water samples. The newly developed sensor shows good reproducibility with RSD of 3.92%. The nylon 6,6 modified SPE showed itself as promising sensor with good selectivity for chlorothalonil determination.
The voltammetric determination of metsulfuron-methyl, a type of pesticide, was investigated on a hanging mercury drop electrode using a differential pulse cathodic stripping voltammetry technique. The experimental parameters, such as the pH of the Britton-Robinson buffer, accumulation time, accumulation potential and initial potential were optimized for the metsulfuron-methyl determination. A well-defined reduction peak was observed at pH 2.0 to 4.0 in the potential range of -0.75 to -1.0 V. The pH of 2.0 was chosen as the optimum pH due to a good stripping signal of the reduction peak. There were no significant interfering ion effects on the electroanalysis of metsulfuron-methyl. The optimized parameters were then used to determine metsulfuron-methyl in the commercial pesticide Ally. The proposed method was highly sensitive due to the lower limit of determination (0.04 mg/L), being relatively selective, and consisting of good precision. The recovery values achieved were about 93% in water samples for this analysis.
A sensitive and selective gas chromatography with mass spectrometry method was developed for the simultaneous determination of three organophosphorus pesticides, namely, chlorpyrifos, malathion, and diazinon in three different food commodities (milk, apples, and drinking water) employing solid-phase extraction for sample pretreatment. Pesticide extraction from different sample matrices was carried out on Chromabond C18 cartridges using 3.0 mL of methanol and 3.0 mL of a mixture of dichloromethane/acetonitrile (1:1 v/v) as the eluting solvent. Analysis was carried out by gas chromatography coupled with mass spectrometry using selected-ion monitoring mode. Good linear relationships were obtained in the range of 0.1-50 μg/L for chlorpyrifos, and 0.05-50 μg/L for both malathion and diazinon pesticides. Good repeatability and recoveries were obtained in the range of 78.54-86.73% for three pesticides under the optimized experimental conditions. The limit of detection ranged from 0.02 to 0.03 μg/L, and the limit of quantification ranged from 0.05 to 0.1 μg/L for all three pesticides. Finally, the developed method was successfully applied for the determination of three targeted pesticides in milk, apples, and drinking water samples each in triplicate. No pesticide was found in apple and milk samples, but chlorpyrifos was found in one drinking water sample below the quantification level.
Drug discovery is a highly complicated, tedious and potentially rewarding approach associated with great risk. Pharmaceutical companies literally spend millions of dollars to produce a single successful drug. The drug discovery process also need strict compliance to the directions on manufacturing and testing of new drug standards before their release into market. All these regulations created the necessity to develop advanced approaches in drug discovery. The contributions of advanced technologies including high resolution analytical instruments, 3-D biological printing, next-generation sequencing and bioinformatics have made positive impact on drug discovery & development. Fortunately, all these advanced technologies are evolving at the right time when new issues are rising in drug development process. In the present review, we have discussed the role of genomics and advanced analytical techniques in drug discovery. Further, we have also discussed the significant advances in drug discovery as case studies.
This paper presents the modelled raindrop size parameters in Skudai region of the Johor Bahru, western Malaysia. Presently, there is no model to forecast the characteristics of DSD in Malaysia, and this has an underpinning implication on wet weather pollution predictions. The climate of Skudai exhibits local variability in regional scale. This study established five different parametric expressions describing the rain rate of Skudai; these models are idiosyncratic to the climate of the region. Sophisticated equipment that converts sound to a relevant raindrop diameter is often too expensive and its cost sometimes overrides its attractiveness. In this study, a physical low-cost method was used to record the DSD of the study area. The Kaplan-Meier method was used to test the aptness of the data to exponential and lognormal distributions, which were subsequently used to formulate the parameterisation of the distributions. This research abrogates the concept of exclusive occurrence of convective storm in tropical regions and presented a new insight into their concurrence appearance.
Rainfall-runoff processes in a small oil palm catchment (8.2 ha) in Johor, Malaysia were examined. Storm hydrographs show rapid responses to rainfall with a short time to peak. The estimated initial hydrologic loss for the oil palm catchment is 5 mm. Despite the low initial loss, the catchment exhibits a high proportion of baseflow, approximately 54% of the total runoff. On an event basis, the stormflow response factor and runoff coefficient ranges from 0.003 to 0.21, and 0.02 to 0.44, respectively. Peakflow and stormflow volume were moderately correlated with rainfall. The hydrographs were satisfactorily modelled using the Hydrologic Engineering Centre-Hydrologic Modelling System (HEC-HMS). The efficiency indexes of the calibration and validation exercises are 0.81 and 0.82, respectively. Based on these preliminary findings, it could be suggested that an oil palm plantation would be able to serve reasonably well in regulating basic hydrological functions.
Runoff quality draining from 17.14 km2 urban catchment in Johor Bahru, Malaysia, was analysed. The land-use consists of residential (30.3%), agricultural (27.3%), open space (27.9%), industrial (8.1%) and commercial (6.4%) areas. Three storm events were sampled in detail. These storms produced stormflow between 0.84 mm and 27.82 mm, and peakflow from 2.19 m3/s to 42.36 m3/s. Water quality showed marked variation during storms especially for TSS, BOD and COD with maximum concentrations of 778 mg/l, 135 mg/l and 358 mg/l, respectively. Concentrations of TOC, DOC, NH3-N, Fe and level of colour were also high. In general, the river quality is badly polluted and falls in Class V based on the Malaysian Interim National Water Quality Standards. Event Mean Concentrations (EMC) for various parameters varied considerably between storms. The largest storm produced higher EMC for TSS, NO3-N and SS whereas the smaller storms tend to register higher EMC for BOD, COD, NH3-N, TOC, Ca, K, Mg, Fe and Zn. Such variations could be explained in terms of pollutant availability and the effects of flushing and dilution. Based on a three-month average recurrence interval (ARI) of rainfall, the estimated event loadings (ton/ha) of TSS, BOD, COD, TOC, NH3-N and NO3-N were 0.055, 0.016, 0.012, 0.039, 0.010, 0.0007 and 0.0002, respectively. Heavy metals present in trace quantities. Storms with 3 months ARI could capture about 70% of the total annual loads of major pollutants.