scholarly journals Optimization of Enzymatic Synthesis of Betulinic Acid Amide in Organic Solvent by Response Surface Methodology (RSM)

2019 ◽  
Vol 19 (4) ◽  
pp. 849
Author(s):  
Nurul Atikah Amin Yusof ◽  
Nursyamsyila Mat Hadzir ◽  
Siti Efliza Ashari ◽  
Nor Suhaila Mohamad Hanapi ◽  
Rossuriati Dol Hamid

Optimization of the lipase catalyzed enzymatic synthesis of betulinic acid amide in the presence of immobilized lipase, Novozym 435 from Candida antartica as a biocatalyst was studied. Response surface methodology (RSM) and 5-level-4-factor central-composite rotatable design (CCRD) were employed to evaluate the effects of the synthesis parameters, such as reaction time (20–36 h), reaction temperature (37–45 °C), substrate molar ratio of betulinic acid to butylamine (1:1–1:3), and enzyme amounts (80–120 mg) on the percentage yield of betulinic acid amide by direct amidation reaction. The optimum conditions for synthesis were: reaction time of 28 h 33 min, reaction temperature of 42.92 °C, substrate molar ratio of 1:2.21, and enzyme amount of 97.77 mg. The percentage yield of actual experimental values obtained 65.09% which compared well with the maximum predicted value of 67.23%. The obtained amide was characterized by GC, GCMS and 13C NMR. Betulinic acid amide (BAA) showed a better cytotoxicity compared to betulinic acid as the concentration inhibited 50% of the cell growth (IC50) against MDA-MB-231 cell line (IC50 < 30 µg/mL).

2016 ◽  
Vol 2016 ◽  
pp. 1-5
Author(s):  
Nurul Atikah Binti Amin Yusof ◽  
Nursyamsyila Mat Hadzir ◽  
Siti Efliza Ashari

Betulinic acid amide was synthesized from the enzymatic reaction of betulinic acid and butylamine catalysed by Novozym 435. The effects of different reaction parameters, such as effect of reaction time, reaction temperature, amount of enzyme, and substrate molar ratio (betulinic acid : butylamine), were studied and conventionally optimised. Based on this study, the enzymatic synthesis of betulinic acid amide was found to be 64.6% at the optimum conditions of 24 h, 40°C, 100 mg enzyme, and 1 : 1 substrate molar ratio in 9 : 1 mixture of chloroform and hexane as solvent. The identification of final product was carried out using TLC, melting point, and FTIR and NMR showed the presence of betulinic acid amide.


2021 ◽  
Vol 29 (4) ◽  
Author(s):  
Ratna Dewi Kusumaningtyas ◽  
Haniif Prasetiawan ◽  
Radenrara Dewi Artanti Putri ◽  
Bayu Triwibowo ◽  
Siti Choirunisa Furi Kurnita ◽  
...  

Nyamplung seed (Calophyllum inophyllum L.) oil is a prospective non-edible vegetable oil as biodiesel feedstock. However, it cannot be directly used in the alkaline catalysed transesterification reaction since it contains high free fatty acid (FFA) of 19.17%. The FFA content above 2% will cause saponification reaction, reducing the biodiesel yield. In this work, FFA removal was performed using sulfuric acid catalysed esterification to meet the maximum FFA amount of 2%. Experimental work and response surface methodology (RSM) analysis were conducted. The reaction was conducted at the fixed molar ratio of nyamplung seed oil and methanol of 1:30 and the reaction times of 120 minutes. The catalyst concentration and the reaction temperature were varied. The highest reaction conversion was 78.18%, and the FFA concentration was decreased to 4.01% at the temperature of 60℃ and reaction time of 120 minutes. The polynomial model analysis on RSM demonstrated that the quadratic model was the most suitable FFA conversion optimisation. The RSM analysis exhibited the optimum FFA conversion of 78.27% and the FFA content of 4%, attained at the reaction temperature, catalyst concentration, and reaction time of 59.09℃, 1.98% g/g nyamplung seed oil, and 119.95 minutes, respectively. Extrapolation using RSM predicted that the targeted FFA content of 2% could be obtained at the temperature, catalyst concentration, and reaction time of 58.97℃, 3%, and 194.9 minutes, respectively, with a fixed molar ratio of oil to methanol of 1:30. The results disclosed that RSM is an appropriate statistical method for optimising the process variable in the esterification reaction to obtain the targeted value of FFA.


2009 ◽  
Vol 12 (13) ◽  
pp. 69-76
Author(s):  
Huong Thi Thanh Le ◽  
Tan Viet Le ◽  
Tan Minh Phan ◽  
Hoa Thi Viet Tran

In this study, biodiesel was produced from fat of tra catfish by methanolysis reaction with KOH/y-A12O3 heterogenous catalyst. This research was carried out using response surface methodology (RSM) based on four-variable central composite design (CCD) with a = 1,54671. The transesterification process variables and their investigated ranges were methanol/fat molar ratio (X1: 7/1 - 9/1), catalyst concentration (X2: 5%-7%), reaction time (X3: 60 min - 120 min), and reaction temperature (X4: 55 °C - 65 °C). The result show the biodiesel yield could be reach up to 92,8 % using the following optimized reaction condition: molar ratio of methanol/fat at 8,26/1, catalyst concentration of 5,79 %, reaction time of 96 min, and reaction temperature at 59,6 °C.


2021 ◽  
Author(s):  
Vaishali Mittal ◽  
Uttam Kumar Ghosh

Abstract Production of biodiesel from microalgae is gaining popularity since it does not compromise food security or the global economy. This article reports biodiesel production with Spirulina microalgae through nanocatalytic transesterification process. The nanocatalyst calcium methoxide Ca(OCH3)2 was synthesized using wet impregnation method and utilized to carry out the transesterification process. The nanocatalyst was characterized to evaluate its structural and spectral characteristics using different characterization techniques such as Thermogravimetric analysis (TGA), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and Brunaeur-Emmett-Teller(BET) measurement for surface area. The result demonstrates that calcium methoxide Ca(OCH3)2 possesses a high catalytic activity compared to a heterogeneous catalyst such as calcium oxide (CaO). The impact of several process parameters such as reaction temperature, the molar ratio of methanol to oil, catalyst concentration, and reaction time used in the transesterification process was optimized by employing central composite design(CCD) based response surface methodology(RSM). The polynomial regression equation of second order was obtained for methyl esters. The model projected a 99% fatty acid methyl esters (FAME) yield for optimal process parameters of reaction time 3hrs,3 wt.% of Ca(OCH3)2 catalyst loading, 80°C reaction temperature, and 30:1 methanol to oil molar ratio.


2011 ◽  
Vol 366 ◽  
pp. 366-369
Author(s):  
Feng Gao ◽  
Rong Fu ◽  
Ming Yang Qian ◽  
Zhu Min Wang ◽  
Xiang Zhang

Response surface methodology was used to optimize the soaking Mg leaching ratio from the boron slurry screened by 25 fractional factorial design. Five effective factors such as H2SO4 concentrations, reaction time, reaction temperature and stir velocity were tested by using 25 fractional factorial design criterion and three effective factors H2SO4 concentrations, reaction time and reaction temperature showed significant effect(P2SO4 concentrations of 0.29mol/l, reaction time of 90 min and reaction temperature of 50°C. Three runs of additional confirmation experiments were conducted. The mixture magnesium leaching value was 58.20%.


2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Yu-Bin Ji ◽  
Fang Dong ◽  
Miao Yu ◽  
Long Qin ◽  
Dan Liu

The response surface methodology was employed to optimize the synthesis conditions of seleno-Sargassum fusiforme(Harv.) Setch. polysaccharide. Three independent variables (reaction time, reaction temperature, and ratio of Na2SeO3to SFPSI) were tested. Furthermore, the characterization and antioxidant activity of Se-SFPSIin vivowere investigated. The result showed that the actual experimental Se content of Se-SFPSI was 3.352 mg/g at the optimum reaction conditions of reaction time 8 h, reaction temperature 71°C, and ratio of Na2SeO3to SFPSIB 1.0 g/g. A series of experiments showed that the characterization of Se-SFPSIB was significantly different from that of SFPSIB. Additionally, antioxidant activity assay indicated that the Se-SFPSIB could increase catalase (CAT), superoxide dismutase (SOD), and glutathione peroxidase (GSH-Px) activity of mice bearing tumor S180in blood, heart, and liver while decreasing malondialdehyde (MDA) levels. It can be concluded that selenylation is a feasible approach to obtain seleno-polysaccharide which was utilized as highly biological medicine or functional food.


2012 ◽  
Vol 622-623 ◽  
pp. 162-165
Author(s):  
Da Wei Yin ◽  
Gang Tao Liang ◽  
Xiao Ming Sun ◽  
Yu Ting Liu

Acetylferrocene was synthesized by acetyl chloride and ferrocene as raw materials, dichloromethane as the solvent, and ZnO as catalyst. Response surface methodology based on three-level, three-variable central composite rotable design was used to evaluate the interactive effects of the ratio of acetyl chloride and ferrocene(2-4), the amount of ZnO(1.0-1.3mol), reaction time(30-60 min)on the percentage yield of acylferrocene. The optimal raw material ratio, amount catalyst, and reaction time was 3:1, 1.19mol, 40min. Under the optimum conditions, the actual experimental yield can reach 86.72%.


Author(s):  
Enmin Lv ◽  
Shaoxuan Ding ◽  
Jie Lu ◽  
Zhuang Li ◽  
Lixiong Du ◽  
...  

Abstract The integration process of polyethersulphone (PES) ultrafiltration with catalytic hydrolysis of lard was optimized by response surface methodology (RSM). The influences of molar ratio of water to lard, reaction time and transmembrane pressure on the fatty acids (FAs) yield were investigated. Results showed that the maximum FAs yield of 99.52 % was obtained under the optimized conditions of molar ratio of water to lard of 6.0:1.0, reaction time of 10.0 h and transmembrane pressure of 100.0 kPa. Moreover, the membrane cleaning efficiency was studied after four cleanings. Furthermore, the kinetic model of membrane separation process was investigated and the activation energy and pre-exponential factor were determined.


2017 ◽  
Vol 2 (1) ◽  
pp. 1-10 ◽  
Author(s):  
O. S. Aliozo ◽  
L. N. Emembolu ◽  
O. D. Onukwuli

Abstract In this research work, melon oil was used as feedstock for methyl ester production. The research was aimed at optimizing the reaction conditions for methyl ester yield from the oil. Response surface methodology (RSM), based on a five level, four variable central composite designs (CCD)was used to optimize and statistically analyze the interaction effect of the process parameter during the biodiesel production processes. A total of 30 experiments were conducted to study the effect of methanol to oil molar ratio, catalyst weight, temperature and reaction time. The optimal yield of biodiesel from melon oil was found to be 94.9% under the following reaction conditions: catalyst weight - 0.8%, methanol to oil molar ratio - 6:1, temperature - 55°C and reaction time of 60mins. The quality of methyl ester produced at these conditions was within the American Society for Testing and Materials (ASTM D6751) specification.


2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Nichaonn Chumuang ◽  
Vittaya Punsuvon

The present study was performed to optimize a heterogeneous calcium methoxide (Ca(OCH3)2) catalyzed transesterification process assisted with tetrahydrofuran (THF) as a cosolvent for biodiesel production from waste cooking oil. Response surface methodology (RSM) with a 5-level-4-factor central composite design was applied to investigate the effect of experimental factors on the percentage of fatty acid methyl ester (FAME) conversion. A quadratic model with an analysis of variance obtained from the RSM is suggested for the prediction of FAME conversion and reveals that 99.43% of the observed variation is explained by the model. The optimum conditions obtained from the RSM were 2.83 wt% of catalyst concentration, 11.6 : 1 methanol-to-oil molar ratio, 100.14 min of reaction time, and 8.65% v/v of THF in methanol concentration. Under these conditions, the properties of the produced biodiesel satisfied the standard requirement. THF as cosolvent successfully decreased the catalyst concentration, methanol-to-oil molar ratio, and reaction time when compared with biodiesel production without cosolvent. The results are encouraging for the application of Ca(OCH3)2 assisted with THF as a cosolvent for environmentally friendly and sustainable biodiesel production.


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