In this study a sensitive and selective gradient reverse phase UPLC-MS/MS method was developed for the simultaneous determination of six process related impurities viz., Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V and Imp-VI in darunavir. The chromatographic separation was performed on Acquity UPLC BEH C18 (50 mm×2.1mm, 1.7μm) column using gradient elution of acetonitrile-methanol (80:20, v/v) and 5.0mM ammonium acetate containing 0.01% formic acid at a flow rate of 0.4mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously using multiple reaction monitoring (MRM) for the quantification of all six impurities in darunavir. The developed method was fully validated following ICH guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness and sample solution stability. The method was able to quantitate Imp-I, Imp-IV, Imp-V at 0.3ppm and Imp-II, Imp-III, and Imp-VI at 0.2ppm with respect to 5.0mg/mL of darunavir. The calibration curves showed good linearity over the concentration range of LOQ to 250% for all six impurities. The correlation coefficient obtained was >0.9989 in all the cases. The accuracy of the method lies between 89.90% and 104.60% for all six impurities. Finally, the method has been successfully applied for three formulation batches of darunavir to determine the above mentioned impurities, however no impurity was found beyond the LOQ. This method is a good quality control tool for the trace level quantification of six process related impurities in darunavir during its synthesis.
Objective: This retrospective study aims to evaluate the possible effects of antihypertensive drugs on alveolar bone loss in patients with chronic periodontitis. Methods: 50 patients on antihypertensive drugs selected as the experimental group and 50 patients with chronic periodontitis with no known systemic illnesses as control group were randomly selected as the study samples. Orthopantomographs were obtained, calibration and assessment of alveolar bone loss was performed by using the computer software program available in the faculty, through radiographic linear measurement procedure. Premolars, first and second molars of both maxilla and mandible were measured from the most apical point to the cementoenamel junction for mesial and distal aspects in the form of millimetres and percentile of the root length. Data was statistically analyzed using independent t-test and Analysis of Covariance in SPSS Version 23 with significance at P-value, p
A new sensing area for a sensor based on surface plasmon resonance (SPR) was fabricated to detect trace amounts of mercury and lead ions. The gold surface used for SPR measurements were modified with polypyrrole-chitosan (PPy-CHI) conducting polymer composite. The polymer layer was deposited on the gold surface by electrodeposition. This optical sensor was used for monitoring toxic metal ions with and without sensitivity enhancement by chitosan in water samples. The higher amounts of resonance angle unit (ΔRU) were obtained for PPy-CHI film due to a specific binding of chitosan with Pb(2+) and Hg(2+) ions. The Pb(2+) ion bind to the polymer films most strongly, and the sensor was more sensitive to Pb(2+) compared to Hg(2+). The concentrations of ions in the parts per million range produced the changes in the SPR angle minimum in the region of 0.03 to 0.07. Data analysis was done by Matlab software using Fresnel formula for multilayer system.
This paper presents the implementing multiple fan beam projection technique using optical fibre sensors for a tomography system. From the dynamic experiment of solid/gas flow using plastic beads in a gravity flow rig, the designed optical fibre sensors are reliable in measuring the mass flow rate below 40% of flow. Another important matter that has been discussed is the image processing rate or IPR. Generally, the applied image reconstruction algorithms, the construction of the sensor and also the designed software are considered to be reliable and suitable to perform real-time image reconstruction and mass flow rate measurements.
Non-small cell lung cancer (NSCLC) incited by epidermal growth factor receptor (EGFR) mutation makes up ∼85% of lung cancer diagnosed and death cases worldwide. The presented study introduced an alternative approach in detecting EGFR mutation using nano-silica integrated with polydimethylsiloxane (PDMS) polymer on interdigitated electrode (IDE) sensor. A 400 μm gap-sized aluminum IDE was modified with nano-polymer layer, which was made up of silica nanoparticles and PDMS polymer. IDE and PDMS-coated IDE (PDMS/IDE) were imaged using electron microscopes that reveals its smooth and ideal sensor morphology. The nano-silica-integrated PDMS/IDE surface was immobilized with EGFR probe and target to specify the lung cancer detection. The sensor specificity was justified through the insignificant current readouts with one-base mismatch and noncomplementary targets. The sensitivity of nano-silica-integrated PDMS/IDE was examined with mutant target spiked in human serum, where the resulting current affirms the detection of EGFR mutation. Based on the slope of the calibration curve, the sensitivity of nano-silica-integrated PDMS/IDE was 2.24E-9 A M-1 . The sensor recognizes EGFR mutation lowest at 1 aM complementary mutant target; however, the detection limit obtained based on 3σ calculation is 10 aM with regression value of 0.97.
This work investigates a new interrogation method of a fiber Bragg grating (FBG) sensor based on longer and shorter wavelengths to distinguish between transversal forces and temperature variations. Calibration experiments were carried out to examine the sensor's repeatability in response to the transversal forces and temperature changes. An automated calibration system was developed for the sensor's characterization, calibration, and repeatability testing. Experimental results showed that the FBG sensor can provide sensor repeatability of 13.21 pm and 17.015 pm for longer and shorter wavelengths, respectively. The obtained calibration coefficients expressed in the linear model using the matrix enabled the sensor to provide accurate predictions for both measurements. Analysis of the calibration and experiment results implied improvements for future work. Overall, the new interrogation method demonstrated the potential to employ the FBG sensing technique where discrimination between two/three measurands is needed.
Climate change-induced spatial and temporal variability of stremflow has significant implications for hydrological processes and water supplies at basin scale. This study investigated the impacts of climate change on streamflow of the Kurau River Basin in Malaysia using a Climate-Smart Decision Support System (CSDSS) to predict future climate sequences. For this, we used 25 reliazations consisting from 10 Global Climate Models (GCMs) and three IPCC Representative Concentration Pathways (RCP4.5, RCP6.0 and RCP8.5). The generated climate sequences were used as input to Soil and Water Assessment Tool (SWAT) to simulate projected changes in hydrological processes in the basin over the period 2021-2080. The model performed fairly well for the Kurau River Basin, with coefficient of determination (R2), Nash-Sutcliffe Efficiency (NSE) and Percent Bias (PBIAS) of 0.65, 0.65 and -3.0, respectively for calibration period (1981-1998) and 0.60, 0.59 and -4.6, respectively for validation period (1996-2005). Future projections over 2021-2080 period show an increase in rainfall during August to January (relatively wet season, called the main irrigation season) but a decrease in rainfall during February to July (relatively dry season, called the off season). Temperature projections show increase in both the maximum and minimum temperatures under the three RCP scenarios, with a maximum increase of 2.5 °C by 2021-2080 relative to baseline period of 1976-2005 under RCP8.5 scenario. The model predicted reduced streamflow under all RCP scenarios compared to the baseline period. Compared to 2021-2050 period, the projected streamflow will be higher during 2051-2080 period by 1.5 m3/s except in February for RCP8.5. The highest streamflow is predicted during August to December for both future periods under RCP8.5. The seasonal changes in streamflow range between -2.8% and -4.3% during the off season, and between 0% (nil) and -3.8% during the main season. The assessment of the impacts of climatic variabilities on the available water resources is necessary to identify adaptation strategies. It is supposed that such assessment on the Kurau River Basin under changing climate would improve operation policy for the Bukit Merah reservoir located at downstream of the basin. Thus, the predicted streamflow of the basin would be of importance to quantify potential impacts of climate change on the Bukit Merah reservoir and to determine the best possible operational strategies for irrigation release.
The authors describe a method for solvent-free mechano-chemical synthesis of a bioinspired sorbent. A 2D ultra-thin carbon sheet similar to graphene oxide was prepared using a natural waste (onion sheet). The formation of 2D carbon sheets was confirmed by Raman spectroscopy, X-ray photoelectron spectroscopy and ATR-IR. The surface morphology was characterized by field emission scanning electron microscopy and high-resolution tunneling electron microscopy. The carbon sheets were decorated with crystalline MnFe2O4 nanoparticles by solid-state reaction at room temperature. The presence of magnetic particles in the final product was confirmed by vibrating sample magnetometry and electron microscopy. The synergistic effect of carbon sheets and MnFe2O4 led to an enhanced sorption of arsenic species compared to bare carbon sheets or to MnFe2O4 nanoparticles. A column was prepared for the simultaneous preconcentration and determination of trace levels of As(III) and As(V) from water samples. The preconcentration factors are between 900 and 833 for As(III) and As(V) species, respectively. The linearity of the calibration plot ranges from 0.4-10 ng mL-1. The detection limits (at 3σ) for both As(III) and As(V) are 30 pg mL-1. The Student's t values for the analysis of spiked samples are lower than the critical Student's t values at a 95% confidence level. The recoveries from spiked water samples range between 99 and 102.8%. Graphical abstract Schematic representation of the preparation of carbon sheets similar to graphene oxide from onion sheaths after pyrolysis at 800 °C. The prepared carbon sheet-MnFe2O4 composite shows excellent arsenic sorption and preconcentration down to the pg mL-1 concentration.
Being an imperative material for man either used as building materials, pottery or as components in material industry and technology, knowledge of clays elemental contents is important. In the present study ten clay samples obtained from various locations in North-West Peninsular Malaysia were used. Majority of the clays were economically manufactured to be used as building materials or pottery. The objective of study was to determine the main elemental contents of the samples, and relate the results to the types of minerals, as well as to compare them with clays from other studies. In the study X-ray Fluorescence (XRF) coupled to samples dilution method and standard calibration samples was used. The elements detected in the study were Si, Al, Fe, Ti, K and Ca. Depending on locations, the percentage concentration ranged between 24.8 – 32.4 for Si, 10.8 – 19.0 for Al, 0.09 – 2.12 for Fe, 0.08 – 1.13 for Ti, 0.45 – 3.39 for K and trace amount of Ca and P. However, Mg that normally found in typical clay was not found in the studied samples. Comparing the oxide of the major elements with other studies, it was found that the clay samples contained mixtures of kaolinite (two-layered structure) and illite (three-layered structure).
Introduction: This study aims to build a standardization method for preparation of effective powder from
FSA and to quantify diosgenin in FSA. Methodology: One kg of FS were used in this study. Setting: BMS, KOM
and KOP, IIUM Kuantan campus. FS were washed with distilled water to exclude any foreign matter, and
were then air dried. FS-powder were put in distilled water in a ratio of 1 g of powder in 20 ml of distilled
water and were shaken at room temperature for 24 hours. Ten mg of hydrolyzed extract sample was diluted
in 10 ml volumetric flask with methanol for 15 minutes. Chromatographic estimation was performed using
an equilibrated reverse phase Eclipse XDB-C18 column (particle size 5 µg, 4.6 mm x 150 mm). Results: One
gram of FSA extract was hydrolyzed to produce sapogenins and 46.6% was recovered. A calibration curve
that was constructed based on five dilutions of diosgenin standard at concentrations of 2, 5, 10, 20, 30 and
50 ppm produced a linear graft (r = 0.999). The concentration of diosgenin in FSA extract as calculated using
the regression analysis was found to be 29.66 µg/ml, 13.81 % w/w on dried weight basis. Conclusion:
Preparation and standardization of effective powder from FSA are the corner stone of many scientific
researches in IIUM and Malaysia. Diosgenin is available in the FSA in adequate concentration. The adequate
amount of diosgenin in the FSA will guide us to do further study in the way of preparation of a natural
product that can be used in the field of reversible anti-fertility therapy.
This paper presents an auto grasping algorithm of a proposed robotic gripper. The purpose is to enhance the grasping mechanism of the gripper. Earlier studies have introduced various methods to enhance the grasping mechanism, but most of the works have not looked at the weight measurement method. Thus, with this algorithm, the weight of the object is calculated based on modified Wheatstone Bridge Circuit (WBC) which is controlled by programmable interface controller (PIC) method. Having this approach introduces and improves the grasping mechanism through an auto grasping algorithm. Experimental results show that an auto grasping algorithm based on pressure sensor measurements leads to a more precise grasping measurement and consequently enhance the sensitivity measurement as well as accurate movement calibration. Furthermore, several different grasping objects based on the proposed method are examined to demonstrate the performance and robustness of our approach.
A simple high-performance liquid chromatography (HPLC) method to determine the content of betulinic acid (BA) in rat plasma collected at different times (0-8 h) after oral administration of Orthosiphon stamineus leaf extract was developed. The features of the assay include protein precipitation using acetonitrile and isocratic elution using reverse phase C-18 column with ultraviolet (UV) detection. The recovery of BA from plasma varied from 98.4 to 102.5%. The R.S.D of intra- and inter-day precision from rat plasma ranged from 4.2 to 9.8%. The maximum concentration of BA in the plasma was 1.2 +/- 0.3 microg/ml at 1 h after oral administration of the extract.
The natural dyes anthocyanin and chlorophyll were extracted from Musa acuminata bracts and Alternanthera dentata leaves, respectively. The dyes were then applied as sensitizers in TiO2-based dye-sensitized solar cells (DSSCs). The ethanol extracts of the dyes had maximum absorbance. High dye yields were obtained under extraction temperatures of 70 to 80°C, and the optimal extraction temperature was approximately 80°C. Moreover, dye concentration sharply decreased under extraction temperatures that exceeded 80°C. High dye concentrations were obtained using acidic extraction solutions, particularly those with a pH value of 4. The DSSC fabricated with anthocyanin from M. acuminata bracts had a conversion efficiency of 0.31%, short-circuit current (Isc) of 0.9mA/cm2, open-circuit voltage (Voc) of 0.58V, and fill factor (FF) of 62.22%. The DSSC sensitized with chlorophyll from A. dentata leaves had a conversion efficiency of 0.13%, Isc of 0.4mA/cm-2,Voc of 0.54V, and FF of 67.5%. The DSSC sensitized with anthocyanin from M. acuminata bracts had a maximum incident photon-to-current conversion efficiency of 42%, which was higher than that of the DSSC sensitized with chlorophyll from A. dentata leaves (23%). Anthocyanin from M. acuminata bracts exhibited the best photosensitization effects.
Groundwater is the main source of water in the Kingdom of Saudi Arabia (KSA). A larger part of groundwater is founded in alluvial (unconfined) aquifers. Prediction of water table elevations in
unconfined aquifers is very useful in water resources planning and management. During the last two
decades, many aquifers in different regions of the KSA experienced significant groundwater decline.
The declines in these aquifers raised concerns over the quantity and quality of groundwater, as well
as concerns over the planning and management policies used in KSA. The main objective of this study was to predict water table fluctuations and to estimate the annual change in water table at an alluvial aquifer at wadi Hada Al Sham near Makkah, KSA. The methodology was achieved using numerical groundwater model (MODFLOW). The model was calibrated and then used to predict water table elevations due to pumping for a period of 5 years. The output of the model was found to be in agreement with the previous records. Moreover, the simulation results also show reasonable declination of water table elevations in the study area during the study period.
Box-Wilson design (BWD) model was applied to determine the optimum values of influencing parameters in anaerobic fermentation to produce hydrogen using Clostridium saccharoperbutylacetonicum N1-4 (ATCC 13564). The main focus of the study was to find the optimal relationship between the hydrogen yield and three variables including initial substrate concentration, initial medium pH and reaction temperature. Microbial growth kinetic parameters for hydrogen production under anaerobic conditions were determined using the Monod model with incorporation of a substrate inhibition term. The values of micro(max) (maximum specific growth rate) and K, (saturation constant) were 0.398 h(-1) and 5.509 g L(-1), respectively, using glucose as the substrate. The experimental substrate and biomass-concentration profiles were in good agreement with those obtained by the kinetic-model predictions. By varying the conditions of the initial substrate concentration (1-40 g L(-1)), reaction temperature (25-40 degrees C) and initial medium pH (4-8), the model predicted a maximum hydrogen yield of 3.24 mol H2 (mol glucose)(-1). The experimental data collected utilising this design was successfully fitted to a second-order polynomial model. An optimum operating condition of 10 g L(-1) initial substrate concentration, 37 degrees C reaction temperature and 6.0 +/- 0.2 initial medium pH gave 80% of the predicted maximum yield of hydrogen where as the experimental yield obtained in this study was 77.75% exhibiting a close accuracy between estimated and experimental values. This is the first report to predict bio-hydrogen yield by applying Box-Wilson Design in anaerobic fermentation while optimizing the effects of environmental factors prevailing there by investigating the effects of environmental factors.
Estimation of the surface dose is very important for patients undergoing radiation therapy. The purpose of this study is to investigate the dose at the surface of a water phantom at a depth of 0.007 cm as recommended by the International Commission on Radiological Protection and International Commission on Radiation Units and Measurement with radiochromic films (RFs), thermoluminescent dosemeters and an ionisation chamber in a 6-MV photon beam. The results were compared with the theoretical calculation using Monte Carlo (MC) simulation software (MCNP5, BEAMnrc and DOSXYZnrc). The RF was calibrated by placing the films at a depth of maximum dose (d(max)) in a solid water phantom and exposing it to doses from 0 to 500 cGy. The films were scanned using a transmission high-resolution HP scanner. The optical density of the film was obtained from the red component of the RGB images using ImageJ software. The per cent surface dose (PSD) and percentage depth dose (PDD) curve were obtained by placing film pieces at the surface and at different depths in the solid water phantom. TLDs were placed at a depth of 10 cm in a solid water phantom for calibration. Then the TLDs were placed at different depths in the water phantom and were exposed to obtain the PDD. The obtained PSD and PDD values were compared with those obtained using a cylindrical ionisation chamber. The PSD was also determined using Monte Carlo simulation of a LINAC 6-MV photon beam. The extrapolation method was used to determine the PSD for all measurements. The PSD was 15.0±3.6% for RF. The TLD measurement of the PSD was 16.0±5.0%. The (0.6 cm(3)) cylindrical ionisation chamber measurement of the PSD was 50.0±3.0%. The theoretical calculation using MCNP5 and DOSXYZnrc yielded a PSD of 15.0±2.0% and 15.7±2.2%. In this study, good agreement between PSD measurements was observed using RF and TLDs with the Monte Carlo calculation. However, the cylindrical chamber measurement yielded an overestimate of the PSD. This is probably due to the ionisation chamber calibration factor that is only valid in charged particle equilibrium condition, which is not achieved at the surface in the build-up region.
Conventional air quality monitoring systems, such as gas analysers, are commonly used in many developed and developing countries to monitor air quality. However, these techniques have high costs associated with both installation and maintenance. One possible solution to complement these techniques is the application of low-cost air quality sensors (LAQSs), which have the potential to give higher spatial and temporal data of gas pollutants with high precision and accuracy. In this paper, we present DiracSense, a custom-made LAQS that monitors the gas pollutants ozone (O₃), nitrogen dioxide (NO₂), and carbon monoxide (CO). The aim of this study is to investigate its performance based on laboratory calibration and field experiments. Several model calibrations were developed to improve the accuracy and performance of the LAQS. Laboratory calibrations were carried out to determine the zero offset and sensitivities of each sensor. The results showed that the sensor performed with a highly linear correlation with the reference instrument with a response-time range from 0.5 to 1.7 min. The performance of several calibration models including a calibrated simple equation and supervised learning algorithms (adaptive neuro-fuzzy inference system or ANFIS and the multilayer feed-forward perceptron or MLP) were compared. The field calibration focused on O₃ measurements due to the lack of a reference instrument for CO and NO₂. Combinations of inputs were evaluated during the development of the supervised learning algorithm. The validation results demonstrated that the ANFIS model with four inputs (WE OX, AE OX, T, and NO₂) had the lowest error in terms of statistical performance and the highest correlation coefficients with respect to the reference instrument (0.8 < r < 0.95). These results suggest that the ANFIS model is promising as a calibration tool since it has the capability to improve the accuracy and performance of the low-cost electrochemical sensor.
This article proposes a set-up for a 3-dimensional ultrasound system using visual probe localization on the conventional 2-dimensional ultrasound machines readily available in most hospitals. A calibrated digital camera is used for probe-tracking (localization) purposes, whereas ultrasound probe calibration is implemented using a purpose-built phantom. The calibration steps and results are detailed here. The overall system is proven effective in clinical trials through scanning of human organs. Results obtained show successful, accurate 3-dimensional representations using this simple cost-effective set-up.
This paper presents the application of TOPMODEL in the Pinang catchment of Malaysia for stream flow simulation. An attempt has been made to use remote-sensing data (ASTER DEM of 30 m resolution) as a primary input for TOPMODEL in order to simulate the stream flow pattern of this tropical catchment. A calibration period was executed based on 2007-2008 hydro-meteorological dataset which gave a satisfactory Nash-Sutcliffe model (NS) model efficiency of 0.749 and a relative volume error (RVE) of -19.2. The recession curve parameter (m) and soil transmissivity at saturation zone (To), were established as the most sensitive parameters through a sensitivity analysis processes. Hydro-meteorological datasets for the period between 2009 and 2010 were used to validate the model which resulted in satisfactory efficiencies of 0.774 (NS) and -19.84 (RVE), respectively. This study demonstrated the ability ASTER DEM acquired from remote sensing to generate the required TOPMODEL parameters for stream flow simulation which gives insights into better management of available water resources.
With associated cure rates in excess of 90%, targeted 131I radioactive iodine therapy has clearly improved thyroid cancer survival. Thus said, potential radiation risks to staff represent a particular concern, current study seeking to determine the radiation exposure of staff from 131I patients during hospitalization, also estimating accumulated dose and related risk to staff during preparation of the radioactive iodine. In present study made over the three-month period 1st February to 1st May 2017, a total of 69 patient treatments were investigated (comprising a cohort of 46 females and 23 males), this being a patient treatment load typically reflective of the workload at the particular centre for such treatments. The patients were administered sodium iodide 131I, retained in capsules containing activities ranging from 370 to 5550 MBq at the time of calibration, radioiodine activity depends on many factors such as gender, clinical indication, body mass index and age. The staff radiation dose arising from each patient treatment was measured on three consecutive days subsequent to capsule administration. In units of µSv, the mean and dose-rates range at distances from the patients of 5 cm, 1 m and 2 m were 209 ± 73 (165-294), 6.8 ± 2 (5.3-9.5) and 0.9 ± 0.3 (0.7-1.2). The annual dose (also measured in units of µSv), based on annual records of doses, for medical physicists, technologists and nurses were 604, 680 and 1000 µSv respectively. In regard to current practice and workload, staff exposures were all found to be below the annual dose limit for radiation workers.