Search results for: lyophilization

Authors: Natalia A. Salazar, Erika K. Méndez, Catalina Álvarez, Carlos E. Orrego

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Lyophilization, also called freeze-drying, is an important dehydration technique mainly used for pharmaceuticals. Food industry also uses lyophilization when it is important to retain most of the nutritional quality, taste, shape and size of dried products and to extend their shelf life. Vacuum-Induced during freezing cycle (VI) has been used in order to control ice nucleation and, consequently, to reduce the time of primary drying cycle of pharmaceuticals preserving quality properties of the final product. This procedure has not been applied in freeze drying of foods. The present work aims to investigate the effect of VI on the lyophilization drying time, final moisture content, density and reconstitutional properties of mango (Mangifera indica L.) slices (MS) and mango pulp-maltodextrin dispersions (MPM) (30% concentration of total solids). Control samples were run at each freezing rate without using induced vacuum. The lyophilization endpoint was the same for all treatments (constant difference between capacitance and Pirani vacuum gauges). From the experimental results it can be concluded that at the high freezing rate (0.4°C/min) reduced the overall process time up to 30% comparing process time required for the control and VI of the lower freeze rate (0.1°C/min) without affecting the quality characteristics of the dried product, which yields a reduction in costs and energy consumption for MS and MPM freeze drying. Controls and samples treated with VI at freezing rate of 0.4°C/min in MS showed similar results in moisture and density parameters. Furthermore, results from MPM dispersion showed favorable values when VI was applied because dried product with low moisture content and low density was obtained at shorter process time compared with the control. There were not found significant differences between reconstitutional properties (rehydration for MS and solubility for MPM) of freeze dried mango resulting from controls, and VI treatments.

Keywords: drying time, lyophilization, mango, vacuum induced freezing

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Authors: Maria Terezinha Santos Leite Neta, Mônica Silva de Jesus, Hannah Caroline Santos Araujo, Rafael Donizete Dutra Sandes, Raquel Anne Ribeiro Dos Santos, Narendra Narain

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Mango is one of the most consumed and appreciated fruits in the world, mainly due to its peculiar and characteristic aroma. Since the fruit is perishable, it requires conservation methods to prolong its shelf life. Mango cubes were dehydrated at 40°C, 50°C and 60°C and by lyophilization, and the effect of these processes was investigated on the physicochemical characteristics (color and texture) of the products and monitoring of the main volatile compounds for the mango aroma. Volatile compounds were extracted by the SPME technique and analyzed in GC-MS system. Drying temperature at 60°C and lyophilization showed higher efficiency in retention of main volatile compounds, being 63.93% and 60.32% of the total concentration present in the fresh pulp, respectively. The freeze-drying process also presented features closer to the fresh mango in relation to color and texture, which contributes to greater acceptability.

Keywords: mango, freeze drying, convection drying, aroma, GC-MS

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Authors: Jaruwan Chutrtong, Tanakwan Bussabun

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Study production of tempeh inoculums powder by freeze-drying comparison with dry at 50°C and the sun bask for developing efficient tempeh inoculums for tempeh producing. Rhizopus oligosporus in PDA slant cultures was incubated at 30°C for 3-5 days until spores and mycelium. Preparation spores suspension with sterilized water and then count the number of started spores. Fill spores suspension in Rice flour and soy flour, mixed with water (in the ratio 10: 7), which is steamed and sterilized at 121°C 15min. Incubated at room temperature for 4 days, count number of spores. Then take the progressive infection and full spore dough to dry at 50°C, sun bask, and lyophilize. Grind to powder. Then pack in plastic bags, stored at 5°C. To investigate quality of inoculums which use different methods, tempeh was fermented every 4 weeks for 24 weeks of the experiment. The result found that rice flour is not suitable to use as raw material in the production of powdered spores. Fungi can growth rarely. Less number of spores and requires more time than soy flour. For drying method, lyophilization is the least possible time. Samples from this method are very hard and very dark and harder to grind than other methods. Drying at 50°C takes longer time than lyophilization but can also set time use for drying. Character of the dry samples is hard solid and brown color, but can be grinded easier. The sun drying takes the longest time, can’t determine the exact time. When the spore powder was used to fermented tempeh immediately, product has similar characters as which use spores that was fresh prepared. The tempeh has normal quality. When spore powder stored at low temperature, tempeh from storage spore in weeks 4, 8 and 12 is still normal. Time spending in production was close to the production of fresh spores. After storage spores for 16 and 20 weeks, tempeh is still normal but growth and sporulation were take longer time than usual (about 6 hours). At 24 week storage, fungal growth is not good, made tempeh looks inferior to normal color, also smell and texture.

Keywords: freez drying, preparation, spores powder, tempeh

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Authors: Alev Yüksel Aydar, Tuncay Yılmaz, Melisa Özçeli̇k, Tuba Aydın, Elif Karabaş

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In this study, response surface methodology (RSM) was used to obtain the optimum conditions for the freeze-drying of Gemlik variety olive seeds of to achieve the desired quality characteristics. The Box Behnken Design (BBD) was applied with three-variable and three replications in the center point. The effects of the different drying parameters including initial temperature of olive seed, pressure and time for freezing on the DPPH activity, total phenolic contents, and oleuropein absorbance value of the samples were investigated. Temperature (50 – 82 °C), pressure (0.2-0.5 mbar), time (6-10 hours) were chosen as independent variables. The analysis revealed that, while the temperature of the product prior to lyophilization and the drying time had no statistically significant effect on DPPH activity (p>0.05), the pressure was more important than the other two variables , and the quadratic effect of pressure had a significant effect on DPPH activity (p<0.05). The R2 and Adj-R2 values of the DPPH activity model were calculated to be 0.8962 and 0.7045, respectively.

Keywords: olive seed, gemlik variety, DPPH, phenolics, optimization

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Authors: Warachate Khobjai, Suriyan Sukati, Khemjira Jarmkom, Pattaranut Eakwaropas, Surachai Techaoei

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The propose of this study was to investigate in vitro thrombolytic activity of Zingiber cassumunar Roxb. and Prasaplai, a Thai herbal formulation of Z. cassumunar Roxb. Herbs were extracted with boiling water and concentrated by lyophilization. To observe their thrombolytic potential, an in vitro clot lysis method was applied where streptokinase and sterile distilled water were used as positive and negative controls, respectively. Crude aqueous extracts from Z. cassumunar Roxb. and Prasaplai formula showed significant thrombolytic activity by clot lysis of 17.90% and 25.21%, respectively, compared to the negative control water (5.16%) while the standard streptokinase revealed 64.78% clot lysis. These findings suggest that Z. cassumunar Roxb. exhibits moderate thrombolytic activity and cloud play an important role in the thrombolytic properties of Prasaplai formula. However, further study should be done to observe in vivo clot dissolving potential and to isolate active component(s) of these extracts.

Keywords: thrombolytic activity, clot lysis, Zingiber cassumunar Roxb., Prasaplai formula, aqueous extract

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Authors: D. C. Soares, J. T. S. Santos, D. G. Costa, A. K. S. Abud, T. P. Nunes, A. V. D. Figueiredo, A. M. de Oliveira Junior

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Mangabeira (Hancornia speciosa Gomes), a native plant in Brazil, is found growing spontaneously in various regions of the country. The high perishability of tropical fruits such as mangaba, causes it to be necessary to use technologies that promote conservation, aiming to increase the shelf life of this fruit and add value. The objective of this study was to compare the mangabas lyophilisation curves behaviours with different sizes and maturation stages. The fruits were freeze-dried for a period of approximately 45 hours at lyophilizer Liotop brand, model L -108. It has been considered large the fruits between 38 and 58 mm diameter and small, between 23 and 28 mm diameter and the two states of maturation, intermediate and mature. Large size mangabas drying curves in both states of maturation were linear behaviour at all process, while the kinetic drying curves related to small fruits, independent of maturation state, had a typical behaviour of drying, with all the well-defined steps. With these results it was noted that the time of lyophilisation was suitable for small mangabas, a fact that did not happen with the larger one. This may indicate that the large mangabas require a longer time to freeze until reaches the equilibrium level, as it happens with the small fruits, going to have constant moisture at the end of the process. For both types of fruit were analysed water activity, acidity, protein, lipid, and vitamin C before and after the process.

Keywords: freeze dryer, mangaba, conservation, chemical characteristics

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Authors: Liliana Zura-Brravo, Antonio Vega-Galvez, Roberto Lemus-Mondaca, Jessica Lopez

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Murta (Ugni molinae T.) is an endemic fruit of Southern Chile, possesses qualities exceptional as its high antioxidants content, that make it increasingly more appreciated for marketing. Dehydration has the potential providing safe food products through the decreased activity water while maintaining their functional properties. The objective of this study was to evaluate the effect of different drying methods on the antioxidant capacity (AC), total flavonoid content (TFC), rehydration indexes and texture the dried murta berry. Five drying technologies were used: convective drying, vacuum drying, sun-air drying, infrared drying and freezing-drying. The antioxidant capacity was measured by the ORAC method, CFT was determined by spectrophotometry, rehydration capacity (CR) and water retention (WHC) by gravimetry, texture profile (TPA) by a texture analyzer TA-XT2 and microstructure by SEM. The results showed that the lyophilized murta had smaller losses AC and TFC with values of 2886.27 routine mg rutin/ 100 g dm and 23359.99 μmol ET/100 g dm, respectively. According to the rehydration indexes, these were affected by the drying methods, where the maximum value of WHC was 92.60 g retained water/100 g sample for the vacuum drying, and the lowest value of CR was 1.43 g water absorbed/g dm for the sun-air drying. Furthermore, the microstructure and TPA showed that lyophilized samples had characteristics similar to the fresh sample. Therefore, it is possible to mention that lyophilization achieved greater extent preserving the characteristics of the murta samples, showing that this method can be used in the food industry and encourage the consumption of dried fruit and thus give it greater added value.

Keywords: antioxidant, drying method, flavonoid, murta berry, texture

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Authors: Kotchamon Yodkhum, Thawatchai Phaechamud

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Hydrophobic chitosan-based materials have been developed as controlled drug delivery system. This study was aimed to prepare and evaluate chitosan-aluminum monostearate composite dispersion (CLA) as fabricating liquid for construct a hydrophobic, controlled-release solid drug delivery matrix. This work was attempted to blend hydrophobic substance, aluminum monostearate (AMS), with chitosan in acidic aqueous medium without using any surfactants or grafting reaction, and high temperature during mixing that are normally performed when preparing hydrophobic chitosan system. Lactic acid solution (2%w/v) was employed as chitosan solvent. CLA dispersion was prepared by dispersing different amounts of AMS (1-20% w/w) in chitosan solution (4% w/w) with continuous agitation using magnetic stirrer for 24 h. Effect of AMS amount on physicochemical properties of the dispersion such as viscosity, rheology and particle size was evaluated. Morphology of chitosan-AMS complex (dispersant) was observed under inverted microscope and atomic force microscope. Stability of CLA dispersions was evaluated after preparation within 48 h. CLA dispersions containing AMS less than 5 % w/w exhibited rheological behavior as Newtonian while that containing higher AMS amount exhibited as pseudoplastic. Particle size of the dispersant was significantly smaller when AMS amount was increased up to 5% w/w and was not different between the higher AMS amount system. Morphology of the dispersant under inverted microscope displayed irregular shape and their size exhibited the same trend with particle size measurement. Observation of the dispersion stability revealed that phase separation occurred faster in the system containing higher AMS amount which indicated lower stability of the system. However, the dispersions were homogeneous and stable more than 12 hours after preparation that enough for fabrication process. The prepared dispersions had ability to be fabricated as a porous matrix via lyophilization technique.

Keywords: chitosan, aluminum monostearate, dispersion, controlled-release

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Authors: Sabine Ambros, Ulrich Kulozik

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Berries such as blue- and raspberries belong to the most valuable fruits. To preserve the characteristic flavor and the high contents of vitamins and anthocyanins, the very sensitive berries are usually dried by lyophilization. As this method is very time- and energy-consuming, the dried fruit is extremely expensive. However, healthy snack foods are growing in popularity. Especially dried fruit free of any additives or additional sugar are more and more asked for. To make these products affordable, the fruits have to be dried by a method that is more energy-efficient than freeze drying but reveals the same high product quality. The additional insertion of microwaves to a freeze drying process was examined in this work to overcome the inconveniences of freeze drying. As microwaves penetrate the product volumetrically, sublimation takes place simultaneously all over the product and leads to a many times shorter process duration. A range of microwave and pressure settings was applied to find the optimum drying condition. The influence of the process parameters microwave power and chamber pressure on drying kinetics, product temperature and product quality was investigated to find the best condition for an energy-efficient process with high product quality. The product quality was evaluated by rehydration capacitiy, crispiness, shrinkage, color, vitamin C content and antioxidative capacity. The conclusion could be drawn that microwave freeze dried berries were almost equal to freeze dried fruit in all measured quality parameters or even could overcome it. Additionally, sensory evaluations could confirm the analytical studies. Drying time could be reduced by more than 75% at much lower energy consumption rates. Thus, an energy-efficient and cost saving method compared to the conventional freeze drying technique for the gentle production of tasty fruit or vegetable snacks has been found. This technique will make dried high-quality snacks available for many of consumers.

Keywords: blueberries, freeze drying, microwave freeze drying, process parameters, product quality

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Authors: Fakhreldin O. Suliman, Alia H. Al-Battashi

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This work explored the interaction of three different imidazoline drugs, naphazoline nitrate (NPH), oxymetazoline hydrochloride (OXY) and xylometazoline hydrochloride (XYL) with two different synthesized cucurbit[n]urils CB[n], cucurbit[7]uril (CB[7]) and cucuribit[8]uril (CB[8]). Three binary inclusion complexes have been investigated in solution and in the solid state. The solid complexes were obtained by lyophilization, whereas the physical mixtures of guests and hosts at a stoichiometric ratio of 1:1 were obtained for each drug. 1HNMR, electrospray ionization mass spectrometry (ESI-MS), and matrix-assisted laser desorption-ionization time-of-flight (MALDI-TOF) mass spectrometry was used to study the complexes prepared in aqueous media. The lyophilized solid complexes were characterized by Fourier transform-infrared spectroscopy (FT-IR), powder X-ray diffractometry (PXRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). MS, FT-IR and PXRD experimental results established in this work reveal that NPH, OXY and XYL molecules form stable inclusion complexes with the two hosts. The TGA and DSC confirmed the enhancement of the thermal stability of each drug and the production of a thermally stable solid complex. The 1HNMR has shown that the protons of the guests faced shifting in ppm and broadening of their peaks upon the formation of inclusion complexes with the selected CB[n]. The aromatic protons of the guest exhibited the highest changes in the chemical shifts and shape of the NMR peaks, suggesting their inclusion into the cavity of the CB[n]. The diffusion coefficients (D), developed from the diffusion-controlled NMR Spectroscopy (DOSY) measurements, for the complexation of the selected imidazoline drugs with CB[7] and CB[8], were decreased in the presence of hosts compared to the free guests indicating the formation of the guest-host adduct. Furthermore, we conducted molecular dynamic simulations and quantum mechanics calculations on these complexes. The results of the theoretical study corroborate the experimental findings and have also shed light on the mechanism of inclusion of the guests into the two hosts. This study generates initial data for potential drug delivery or drug formulation systems for these three selected imidazoline drug compounds based on their inclusion into the CB[n] cavities.

Keywords: cucurbit[n]urils, imidazoline, inclusion complexes, molecular dynamics, DFT calculations, mass spectrometry

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Authors: Yik Sin Chan, Nam Weng Sit, Fook Yee Chye, van Ofwegen Leen, de Voogd Nicole, Kong Soo Khoo

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Chikungunya fever is an arboviral disease transmitted by the Aedes mosquitoes. It has resulted in epidemics of the disease in tropical countries in the Indian Ocean and South East Asian regions. The recent spread of this disease to the temperate countries such as France and Italy, coupled with the absence of vaccines and effective antiviral drugs make chikungunya fever a worldwide health threat. This study aims to investigate the anti-chikungunya virus activity of selected marine organism samples collected from Malaysian coastal areas, including seaweeds (Caulerpa racemosa, Caulerpa sertularioides and Kappaphycus alvarezii), a soft coral (Lobophytum microlobulatum) and a sponge (Spheciospongia vagabunda). Following lyophilization (oven drying at 40C for K. alvarezii) and grinding to powder form, each sample was subjected to sequential solvent extraction using hexane, chloroform, ethyl acetate, ethanol, methanol and distilled water in order to extract bioactive compounds. The antiviral activity was evaluated using monkey kidney epithelial (Vero) cells infected with the virus (multiplicity of infection=1). The cell viability was determined by Neutral Red uptake assay. 70% of the 30 extracts showed weak inhibitory activity with cell viability ≤30%. Seven of the extracts exhibited moderate inhibitory activity (cell viability: 31%-69%). These were the chloroform, ethyl acetate, ethanol and methanol extracts of C. racemosa; chloroform and ethyl acetate extracts of L. microlobulatum; and the chloroform extract of C. sertularioides. Only the hexane and ethanol extracts of L. microlobulatum showed strong inhibitory activity against the virus, resulting in cell viabilities (mean±SD; n=3) of 73.3±2.6% and 79.2±0.9%, respectively. The corresponding mean 50% effective concentrations (EC50) for the extracts were 14.2±0.2 and 115.3±1.2 µg/mL, respectively. The ethanol extract of the soft coral L. microlobulatum appears to hold the most promise for further characterization of active principles as it possessed greater selectivity index (SI>5.6) compared to the hexane extract (SI=2.1).

Keywords: antiviral, seaweed, sponge, soft coral, vero cell

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Authors: Elizalde D. Bana

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Healing restores continuity and form through cell replication; hence, conserving structural integrity. In response to the worldwide pressing problem of chronic wounds in the healthcare delivery system, the researcher aims to provide effective intervention to preserve the structural integrity of the person. The wound healing effects of cryopreserved and lyophilized amniotic membrane (AM) of a term fetus embedded into two (2) concentrations (1.5 % and 1.0 %) of absorption-based ointment has been evaluated in vivo using the excision wound healing model 1x1 cm size. The total protein concentration in full term fetus was determined by the Biuret and Bradford methods, which are based on UV-visible spectroscopy. The percentages of protein presence in 9.5 mg (Mass total sample) of Amniotic membrane ranges between 14.77 – 14.46 % in Bradford method, while slightly lower to 13.78 – 13.80 % concentration in Biuret method, respectively. Bradford method evidently showed higher sensitivity for proteins than Biuret test. Overall, the amniotic membrane is composed principally of proteins in which a copious amount of literature substantially proved its healing abilities. After which, an area of 1 cm by 1 cm skin tissue was excised to its full thickness from the dorsolateral aspect of the isogenic mice and was applied twice a day with the ointment formulation having two (2) concentrations for the diabetic group and non-diabetic group. The wounds of each animal were left undressed and its area was measured every other day by a standard measurement formula from day 2,4,6,8,10,12 and 14. By the 14th day, the ointment containing 1.5 % of AM in absorption-based ointment applied to non-diabetic and diabetic group showed 100 % healing. The wound areas in the animals treated with the standard antibiotic, Mupirocin Ointment (Brand X) showed a 100% healing by the 14th day but with traces of scars, indicating that AM prepared from cryopreservation and lyophilization, at that given concentration, had a better wound healing property than the standard antibiotic. Four (4) multivariate tests were used which showed a significant interaction between days and treatments, meaning that the ointments prepared in two differing concentrations and induced in different groups of the mice had a significant effect on the percent of contraction over time. Furthermore, the evaluations of its effectiveness to wound healing were all significant although in differing degrees. It is observed that the higher the concentrations of amniotic membrane, the more effective are the results.

Keywords: wounds, healing, amniotic membrane ointments, biomedical, stem cell

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Authors: Aipeng Zhu, Yun Zhang

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The growing grievous environment problems together with the exhaustion of energy resources put urgent demands for developing high energy density. Considering the factors including capacity, resource and environment, Manganese-based lithium-rich layer-structured cathode materials xLi₂MnO₃⋅(1-x)LiMO₂ (M = Ni, Co, Mn, and other metals) are drawing increasing attention due to their high reversible capacities, high discharge potentials, and low cost. They are expected to be one type of the most promising cathode materials for the next-generation Li-ion batteries (LIBs) with higher energy densities. Unfortunately, their commercial applications are hindered with crucial drawbacks such as poor rate performance, limited cycle life and continuous falling of the discharge potential. With decades of extensive studies, significant achievements have been obtained in improving their cyclability and rate performances, but they cannot meet the requirement of commercial utilization till now. One major problem for lithium-rich layer-structured cathode materials (LLOs) is the side reaction during cycling, which leads to severe surface degradation. In this process, the metal ions can dissolve in the electrolyte, and the surface phase change can hinder the intercalation/deintercalation of Li ions and resulting in low capacity retention and low working voltage. To optimize the LLOs cathode material, the surface coating is an efficient method. Considering the price and stability, Al₂O₃ was used as a coating material in the research. Meanwhile, due to the low initial Coulombic efficiency (ICE), the pristine LLOs was pretreated by KMnO₄ to increase the ICE. The precursor was prepared by a facile coprecipitation method. The as-prepared precursor was then thoroughly mixed with Li₂CO₃ and calcined in air at 500℃ for 5h and 900℃ for 12h to produce Li₁.₂[Ni₀.₂Mn₀.₆]O₂ (LNMO). The LNMO was then put into 0.1ml/g KMnO₄ solution stirring for 3h. The resultant was filtered and washed with water, and dried in an oven. The LLOs obtained was dispersed in Al(NO₃)₃ solution. The mixture was lyophilized to confer the Al(NO₃)₃ was uniformly coated on LLOs. After lyophilization, the LLOs was calcined at 500℃ for 3h to obtain LNMO@LMO@ALO. The working electrodes were prepared by casting the mixture of active material, acetylene black, and binder (polyvinglidene fluoride) dissolved in N-methyl-2-pyrrolidone with a mass ratio of 80: 15: 5 onto an aluminum foil. The electrochemical performance tests showed that the multiple surface modified materials had a higher initial Coulombic efficiency (84%) and better capacity retention (91% after 100 cycles) compared with that of pristine LNMO (76% and 80%, respectively). The modified material suggests that the KMnO₄ pretreat and Al₂O₃ coating can increase the ICE and cycling stability.

Keywords: Li-rich materials, surface coating, lithium ion batteries, Al₂O₃

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