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Fulltext Optimisation and Characterisation of Lipase-Catalysed Synthesis of a Kojic Monooleate Ester in a Solvent-Free System by Response Surface Methodology

Jumbri K, Al-Haniff Rozy MF, Ashari SE, Mohamad R, Basri M, Fard Masoumi HR

PLoS One, 2015;10(12):e0144664.
PMID: 26657030 DOI: 10.1371/journal.pone.0144664

Kojic acid is widely used to inhibit the browning effect of tyrosinase in cosmetic and food industries. In this work, synthesis of kojic monooleate ester (KMO) was carried out using lipase-catalysed esterification of kojic acid and oleic acid in a solvent-free system. Response Surface Methodology (RSM) based on central composite rotatable design (CCRD) was used to optimise the main important reaction variables, such as enzyme amount, reaction temperature, substrate molar ratio, and reaction time along with immobilised lipase from Candida Antarctica (Novozym 435) as a biocatalyst. The RSM data indicated that the reaction temperature was less significant in comparison to other factors for the production of a KMO ester. By using this statistical analysis, a quadratic model was developed in order to correlate the preparation variable to the response (reaction yield). The optimum conditions for the enzymatic synthesis of KMO were as follows: an enzyme amount of 2.0 wt%, reaction temperature of 83.69°C, substrate molar ratio of 1:2.37 (mmole kojic acid:oleic acid) and a reaction time of 300.0 min. Under these conditions, the actual yield percentage obtained was 42.09%, which is comparably well with the maximum predicted value of 44.46%. Under the optimal conditions, Novozym 435 could be reused for 5 cycles for KMO production percentage yield of at least 40%. The results demonstrated that statistical analysis using RSM can be used efficiently to optimise the production of a KMO ester. Moreover, the optimum conditions obtained can be applied to scale-up the process and minimise the cost.
Fulltext Comparison of process parameter optimization using different designs in nanoemulsion-based formulation for transdermal delivery of fullerene

Ngan CL, Basri M, Lye FF, Fard Masoumi HR, Tripathy M, Karjiban RA, et al.

Int J Nanomedicine, 2014;9:4375-86.
PMID: 25258528 DOI: 10.2147/IJN.S65689

This research aims to formulate and to optimize a nanoemulsion-based formulation containing fullerene, an antioxidant, stabilized by a low amount of mixed surfactants using high shear and the ultrasonic emulsification method for transdermal delivery. Process parameters optimization of fullerene nanoemulsions was done by employing response surface methodology, which involved statistical multivariate analysis. Optimization of independent variables was investigated using experimental design based on Box-Behnken design and central composite rotatable design. An investigation on the effect of the homogenization rate (4,000-5,000 rpm), sonication amplitude (20%-60%), and sonication time (30-150 seconds) on the particle size, ζ-potential, and viscosity of the colloidal systems was conducted. Under the optimum conditions, the central composite rotatable design model suggested the response variables for particle size, ζ-potential, and viscosity of the fullerene nanoemulsion were 152.5 nm, -52.6 mV, and 44.6 pascal seconds, respectively. In contrast, the Box-Behnken design model proposed that preparation under the optimum condition would produce nanoemulsion with particle size, ζ-potential, and viscosity of 148.5 nm, -55.2 mV, and 39.9 pascal seconds, respectively. The suggested process parameters to obtain optimum formulation by both models yielded actual response values similar to the predicted values with residual standard error of <2%. The optimum formulation showed more elastic and solid-like characteristics due to the existence of a large linear viscoelastic region.
Fulltext Rapid adsorption of copper(II) and lead(II) by rice straw/Fe₃O₄ nanocomposite: optimization, equilibrium isotherms, and adsorption kinetics study

Khandanlou R, Ahmad MB, Fard Masoumi HR, Shameli K, Basri M, Kalantari K

PLoS One, 2015;10(3):e0120264.
PMID: 25815470 DOI: 10.1371/journal.pone.0120264

Rice straw/magnetic nanocomposites (RS/Fe3O4-NCs) were prepared via co-precipitation method for removal of Pb(II) and Cu(II) from aqueous solutions. Response surface methodology (RSM) was utilized to find the optimum conditions for removal of ions. The effects of three independent variables including initial ion concentration, removal time, and adsorbent dosage were investigated on the maximum adsorption of Pb (II) and Cu (II). The optimum conditions for the adsorption of Pb(II) and Cu(II) were obtained (100 and 60 mg/L) of initial ion concentration, (41.96 and 59.35 s) of removal time and 0.13 g of adsorbent for both ions, respectively. The maximum removal efficiencies of Pb(II) and Cu(II) were obtained 96.25% and 75.54%, respectively. In the equilibrium isotherm study, the adsorption data fitted well with the Langmuir isotherm model. The adsorption kinetics was best depicted by the pseudo-second order model. Desorption experiments showed adsorbent can be reused successfully for three adsorption-desorption cycles.
Fulltext An Artificial Neural Network Based Analysis of Factors Controlling Particle Size in a Virgin Coconut Oil-Based Nanoemulsion System Containing Copper Peptide

Samson S, Basri M, Fard Masoumi HR, Abdul Malek E, Abedi Karjiban R

PLoS One, 2016;11(7):e0157737.
PMID: 27383135 DOI: 10.1371/journal.pone.0157737

A predictive model of a virgin coconut oil (VCO) nanoemulsion system for the topical delivery of copper peptide (an anti-aging compound) was developed using an artificial neural network (ANN) to investigate the factors that influence particle size. Four independent variables including the amount of VCO, Tween 80: Pluronic F68 (T80:PF68), xanthan gum and water were the inputs whereas particle size was taken as the response for the trained network. Genetic algorithms (GA) were used to model the data which were divided into training sets, testing sets and validation sets. The model obtained indicated the high quality performance of the neural network and its capability to identify the critical composition factors for the VCO nanoemulsion. The main factor controlling the particle size was found out to be xanthan gum (28.56%) followed by T80:PF68 (26.9%), VCO (22.8%) and water (21.74%). The formulation containing copper peptide was then successfully prepared using optimum conditions and particle sizes of 120.7 nm were obtained. The final formulation exhibited a zeta potential lower than -25 mV and showed good physical stability towards centrifugation test, freeze-thaw cycle test and storage at temperature 25°C and 45°C.
Fulltext Modeling and optimization of nanoemulsion containing Sorafenib for cancer treatment by response surface methodology

Izadiyan Z, Basri M, Fard Masoumi HR, Abedi Karjiban R, Salim N, Shameli K

Chem Cent J, 2017;11:21.
PMID: 28293282 DOI: 10.1186/s13065-017-0248-6

The aim of this study is the development of nanoemulsions for intravenous administration of Sorafenib, which is a poorly soluble drug with no parenteral treatment. The formulation was prepared by a high energy emulsification method and optimized by response surface methodology. The effects of overhead stirring time, high shear rate, high shear time, and cycles of high-pressure homogenizer were studied in the preparation of nanoemulsion loaded with Sorafenib. Most of the particles in nanoemulsion are spherical in shape, the smallest particle size being 82.14 nm. The results of the 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide, a tetrazole reveal that the optimum formulation does not affect normal cells significantly in low drug concentrations but could remove the cancer cells. Finally, a formulation containing Sorafenib retained its properties over a period of 90 days. With characterization, the study of the formulated nanoemulsion has the potential to be used as a parenteral nanoemulsion in the treatment of cancer. Graphical abstractSchematic figure of high pressure homogenizer device.
Fulltext Enhancement of physicochemical properties of nanocolloidal carrier loaded with cyclosporine for topical treatment of psoriasis: in vitro diffusion and in vivo hydrating action

Musa SH, Basri M, Fard Masoumi HR, Shamsudin N, Salim N

Int J Nanomedicine, 2017;12:2427-2441.
PMID: 28405165 DOI: 10.2147/IJN.S125302

Psoriasis is a chronic autoimmune disease that cannot be cured. It can however be controlled by various forms of treatment, including topical, systemic agents, and phototherapy. Topical treatment is the first-line treatment and favored by most physicians, as this form of therapy has more patient compliance. Introducing a nanoemulsion for transporting cyclosporine as an anti-inflammatory drug to an itchy site of skin disease would enhance the effectiveness of topical treatment for psoriasis. The addition of nutmeg and virgin coconut-oil mixture, with their unique properties, could improve cyclosporine loading and solubility. A high-shear homogenizer was used in formulating a cyclosporine-loaded nanoemulsion. A D-optimal mixture experimental design was used in the optimization of nanoemulsion compositions, in order to understand the relationships behind the effect of independent variables (oil, surfactant, xanthan gum, and water content) on physicochemical response (particle size and polydispersity index) and rheological response (viscosity and k-value). Investigation of these variables suggests two optimized formulations with specific oil (15% and 20%), surfactant (15%), xanthan gum (0.75%), and water content (67.55% and 62.55%), which possessed intended responses and good stability against separation over 3 months' storage at different temperatures. Optimized nanoemulsions of pH 4.5 were further studied with all types of stability analysis: physical stability, coalescence-rate analysis, Ostwald ripening, and freeze-thaw cycles. In vitro release proved the efficacy of nanosize emulsions in carrying cyclosporine across rat skin and a synthetic membrane that best fit the Korsmeyer-Peppas kinetic model. In vivo skin analysis towards healthy volunteers showed a significant improvement in the stratum corneum in skin hydration.
Phytoremediation of palm oil mill secondary effluent (POMSE) by Chrysopogon zizanioides (L.) using artificial neural networks

Darajeh N, Idris A, Fard Masoumi HR, Nourani A, Truong P, Rezania S

Int J Phytoremediation, 2017 May 04;19(5):413-424.
PMID: 27748626 DOI: 10.1080/15226514.2016.1244159

Artificial neural networks (ANNs) have been widely used to solve the problems because of their reliable, robust, and salient characteristics in capturing the nonlinear relationships between variables in complex systems. In this study, ANN was applied for modeling of Chemical Oxygen Demand (COD) and biodegradable organic matter (BOD) removal from palm oil mill secondary effluent (POMSE) by vetiver system. The independent variable, including POMSE concentration, vetiver slips density, and removal time, has been considered as input parameters to optimize the network, while the removal percentage of COD and BOD were selected as output. To determine the number of hidden layer nodes, the root mean squared error of testing set was minimized, and the topologies of the algorithms were compared by coefficient of determination and absolute average deviation. The comparison indicated that the quick propagation (QP) algorithm had minimum root mean squared error and absolute average deviation, and maximum coefficient of determination. The importance values of the variables was included vetiver slips density with 42.41%, time with 29.8%, and the POMSE concentration with 27.79%, which showed none of them, is negligible. Results show that the ANN has great potential ability in prediction of COD and BOD removal from POMSE with residual standard error (RSE) of less than 0.45%.
Improvement of physicochemical properties of nanocolloidal carrier loaded with low water solubility drug for parenteral cancer treatment by Response Surface Methodology

Izadiyan Z, Basri M, Fard Masoumi HR, Abedi Karjiban R, Salim N, Kalantari K

Mater Sci Eng C Mater Biol Appl, 2019 Jan 01;94:841-849.
PMID: 30423770 DOI: 10.1016/j.msec.2018.10.015

Nanoemulsions have been used as a drug carrier system, particularly for poorly water-soluble drugs. Sorafenib is a poorly soluble drug and also there is no parenteral treatment. The aim of this study is the development of nanoemulsions for intravenous administration of Sorafenib. The formulations were prepared by high energy emulsification method and optimized by using Response Surface Methodology (RSM). Here, the effect of independent composition variables of lecithin (1.16-2.84%, w/w), Medium-Chain Triglycerides (2.32-5.68%, w/w) and polysorbate 80 (0.58-1.42%, w/w) amounts on the properties of Sorafenib-loaded nanoemulsion was investigated. The three responses variables were particle size, zeta potential, and polydispersity index. Optimization of the conditions according to the three dependent variables was performed for the preparation of the Sorafenib-loaded nanoemulsions with the minimum value of particle size, suitable rage of zeta potential, and polydispersity index. A formulation containing 0.05% of Sorafenib kept its properties in a satisfactory range over the evaluated period. The composition with 3% Medium-Chain Triglycerides, 2.5% lecithin and 1.22% polysorbate 80 exhibited the smallest particle size and polydispersity index (43.17 nm and 0.22, respectively) with the zeta potential of -38.8 mV was the optimized composition. The fabricated nanoemulsion was characterized by the transmission electron microscope (TEM), viscosity, and stability assessment study. Also, the cytotoxicity result showed that the optimum formulations had no significant effect on a normal cell in a low concentration of the drug but could eliminate the cancer cells. The dose-dependent toxicity made it a suitable candidate for parenteral applications in the treatment of breast cancer. Furthermore, the optimized formulation indicated good storage stability for 3 months at different temperatures (4 ± 2 °C, 25 ± 2 °C and 45 ± 2 °C).
Fulltext Effects of temperature, time, and solvent ratio on the extraction of phenolic compounds and the anti-radical activity of Clinacanthus nutans Lindau leaves by response surface methodology

Che Sulaiman IS, Basri M, Fard Masoumi HR, Chee WJ, Ashari SE, Ismail M

Chem Cent J, 2017 Jun 14;11(1):54.
PMID: 29086900 DOI: 10.1186/s13065-017-0285-1

BACKGROUND: Clinacanthus nutans Lindau is a well-known plant, native to tropical Asian countries. Reports on this plant that is rich in phenolic compounds have focused on its therapeutic anti-inflammatory, anti-herpes simplex, antioxidant, and anti-cancer characteristics. In this paper, the influence of the extraction parameters-temperatures (60-80 °C), times (80-120 min), and solvent ratios (70:30-90:10) of water:ethanol were investigated using response surface methodology in order to determine the optimum extraction conditions that could produce maximum extraction yields of the phenolic compounds and the highest anti-radical activity of the C. nutans extract.
RESULTS: The optimum conditions suggested by the predicted model were: an extraction temperature of 60 °C, an extraction time of 120 min and a water:ethanol solvent ratio of 90:10 v/v%. The residual standard error of 0.2% indicated that there was no significant difference between the actual and predicted values and it proved that the models were adequate to predict the relevant responses. All the independent variables had a significant effect (p
Modeling BOD and COD removal from Palm Oil Mill Secondary Effluent in floating wetland by Chrysopogon zizanioides (L.) using response surface methodology

Darajeh N, Idris A, Fard Masoumi HR, Nourani A, Truong P, Sairi NA

J Environ Manage, 2016 Oct 01;181:343-352.
PMID: 27393941 DOI: 10.1016/j.jenvman.2016.06.060

While the oil palm industry has been recognized for its contribution towards economic growth and rapid development, it has also contributed to environmental pollution due to the production of huge quantities of by-products from the oil extraction process. A phytoremediation technique (floating Vetiver system) was used to treat Palm Oil Mill Secondary Effluent (POMSE). A batch study using 40 L treatment tanks was carried out under different conditions and Response Surface Methodology (RSM) was applied to optimize the treatment process. A three factor central composite design (CCD) was used to predict the experimental variables (POMSE concentration, Vetiver plant density and time). An extraordinary decrease in organic matter as measured by BOD and COD (96% and 94% respectively) was recorded during the experimental duration of 4 weeks using a density of 30 Vetiver plants. The best and lowest final BOD of 2 mg/L was obtained when using 15 Vetiver plants after 13 days for low concentration POMSE (initial BOD = 50 mg/L). The next best result of BOD at 32 mg/L was obtained when using 30 Vetiver plants after 24 days for medium concentration POMSE (initial BOD = 175 mg/L). These results confirmed the validity of the model, and the experimental value was determined to be quite close to the predicted value, implying that the empirical model derived from RSM experimental design can be used to adequately describe the relationship between the independent variables and response. The study showed that the Vetiver system is an effective method of treating POMSE.
Fulltext Enhancing the Bioconversion of Azelaic Acid to Its Derivatives by Response Surface Methodology

Khairudin N, Basri M, Fard Masoumi HR, Samson S, Ashari SE

Molecules, 2018 Feb 13;23(2).
PMID: 29438284 DOI: 10.3390/molecules23020397

Azelaic acid (AzA) and its derivatives have been known to be effective in the treatment of acne and various cutaneous hyperpigmentary disorders. The esterification of azelaic acid with lauryl alcohol (LA) to produce dilaurylazelate using immobilized lipase B from Candida antarctica (Novozym 435) is reported. Response surface methodology was selected to optimize the reaction conditions. A well-fitting quadratic polynomial regression model for the acid conversion was established with regards to several parameters, including reaction time and temperature, enzyme amount, and substrate molar ratios. The regression equation obtained by the central composite design of RSM predicted that the optimal reaction conditions included a reaction time of 360 min, 0.14 g of enzyme, a reaction temperature of 46 °C, and a molar ratio of substrates of 1:4.1. The results from the model were in good agreement with the experimental data and were within the experimental range (R² of 0.9732).The inhibition zone can be seen at dilaurylazelate ester with diameter 9.0±0.1 mm activities against Staphylococcus epidermidis S273. The normal fibroblasts cell line (3T3) was used to assess the cytotoxicity activity of AzA and AzA derivative, which is dilaurylazelate ester. The comparison of the IC50 (50% inhibition of cell viability) value for AzA and AzA derivative was demonstrated. The IC50 value for AzA was 85.28 μg/mL, whereas the IC50 value for AzA derivative was more than 100 μg/mL. The 3T3 cell was still able to survive without any sign of toxicity from the AzA derivative; thus, it was proven to be non-toxic in this MTT assay when compared with AzA.
Fulltext Enhanced biocatalytic esterification with lipase-immobilized chitosan/graphene oxide beads

Lau SC, Lim HN, Basri M, Fard Masoumi HR, Ahmad Tajudin A, Huang NM, et al.

PLoS One, 2014;9(8):e104695.
PMID: 25127038 DOI: 10.1371/journal.pone.0104695

In this work, lipase from Candida rugosa was immobilized onto chitosan/graphene oxide beads. This was to provide an enzyme-immobilizing carrier with excellent enzyme immobilization activity for an enzyme group requiring hydrophilicity on the immobilizing carrier. In addition, this work involved a process for the preparation of an enzymatically active product insoluble in a reaction medium consisting of lauric acid and oleyl alcohol as reactants and hexane as a solvent. This product enabled the stability of the enzyme under the working conditions and allowed the enzyme to be readily isolated from the support. In particular, this meant that an enzymatic reaction could be stopped by the simple mechanical separation of the "insoluble" enzyme from the reaction medium. Chitosan was incorporated with graphene oxide because the latter was able to enhance the physical strength of the chitosan beads by its superior mechanical integrity and low thermal conductivity. The X-ray diffraction pattern showed that the graphene oxide was successfully embedded within the structure of the chitosan. Further, the lipase incorporation on the beads was confirmed by a thermo-gravimetric analysis. The lipase immobilization on the beads involved the functionalization with coupling agents, N-hydroxysulfosuccinimide sodium (NHS) and 1-ethyl-(3-dimethylaminopropyl) carbodiimide (EDC), and it possessed a high enzyme activity of 64 U. The overall esterification conversion of the prepared product was 78% at 60 °C, and it attained conversions of 98% and 88% with commercially available lipozyme and novozyme, respectively, under similar experimental conditions.
Fulltext Semi-empirical study of ortho-cresol photo degradation in manganese-doped zinc oxide nanoparticles suspensions

Abdollahi Y, Zakaria A, Abdullah AH, Fard Masoumi HR, Jahangirian H, Shameli K, et al.

Chem Cent J, 2012 Aug 21;6(1):88.
PMID: 22909072 DOI: 10.1186/1752-153X-6-88

The optimization processes of photo degradation are complicated and expensive when it is performed with traditional methods such as one variable at a time. In this research, the condition of ortho-cresol (o-cresol) photo degradation was optimized by using a semi empirical method. First of all, the experiments were designed with four effective factors including irradiation time, pH, photo catalyst's amount, o-cresol concentration and photo degradation % as response by response surface methodology (RSM). The RSM used central composite design (CCD) method consists of 30 runs to obtain the actual responses. The actual responses were fitted with the second order algebraic polynomial equation to select a model (suggested model). The suggested model was validated by a few numbers of excellent statistical evidences in analysis of variance (ANOVA). The used evidences include high F-value (143.12), very low P-value (<0.0001), non-significant lack of fit, the determination coefficient (R2 = 0.99) and the adequate precision (47.067). To visualize the optimum, the validated model simulated the condition of variables and response (photo degradation %) be using a few number of three dimensional plots (3D). To confirm the model, the optimums were performed in laboratory. The results of performed experiments were quite close to the predicted values. In conclusion, the study indicated that the model is successful to simulate the optimum condition of o-cresol photo degradation under visible-light irradiation by manganese doped ZnO nanoparticles.

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