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1.
Food Chem X ; 24: 101790, 2024 Dec 30.
Article in English | MEDLINE | ID: mdl-39296481

ABSTRACT

Plums (Prunus salicina and Prunus domestica) are prevalent in southwestern China, and have attracted interest owing to their delectable taste and exceptional nutritional properties. Therefore, this study aimed to investigate the nutritional and flavor properties of plum to improve its nutritional utilization. Specifically, we determined the soluble sugars, organic acids, and phenolic components in 86 accessions using high-performance liquid chromatography. Notably, glucose, fructose, malic, and quinic acids were the predominant sweetness and acidity in plums, with sucrose contributing more to the sweetness of the flesh than the peel. Moreover, The peel contains 5.5 fold more phenolics than flesh, epicatechin, gallic acid, and proanthocyanidins C1 and B2 were the primary sources of astringency. Correlation and principal component analyses showed eight core factors for plum flavor rating, and a specific rating criterion was established. Conclusively, these findings provide information on the integrated flavor evaluation criteria and for enhancing optimal breeding of plums.

2.
Food Chem ; 454: 139749, 2024 Oct 01.
Article in English | MEDLINE | ID: mdl-38797104

ABSTRACT

Plastic food packaging, with its harmful migration of microplastics and nanoplastics into food, presents significant ecological imbalance and human health risks. In this regard, using food and agricultural byproducts as packaging materials reduces environmental and economic concerns and supports their sustainable management. Herein, cellulosic residue from corncob was employed as a renewable source for developing biodegradable packaging films. It was solubilized in ZnCl2 solution, crosslinked with Ca2+ ions, and plasticized with sorbitol to form films and used to improve the shelf-life of raspberries. The optimized film possesses water vapor permeability, tensile strength, and elongation at break of 1.8(4) x10-10 g-1 s-1 Pa-1, 4.7(1) MPa, and 15.4(7)%, respectively. It displays UV-blocking and antioxidant properties and biodegrades within 29 days at 24% soil moisture. It preserves raspberries for 7 and 5 more days at room temperature and refrigeration conditions, respectively, compared to polystyrene film. Overall, more value addition could be envisioned from agricultural residues to minimize post-harvest losses and food waste through biodegradable packaging, which also aids in mitigating plastic perils.


Subject(s)
Food Packaging , Food Preservation , Rubus , Food Packaging/instrumentation , Rubus/chemistry , Food Preservation/methods , Food Preservation/instrumentation , Permeability , Tensile Strength , Biodegradable Plastics/chemistry , Biodegradation, Environmental , Fruit/chemistry , Cellulose/chemistry
3.
Food Chem ; 441: 138258, 2024 May 30.
Article in English | MEDLINE | ID: mdl-38219359

ABSTRACT

The purpose of this study was to compare the influences of gamma-poly glutamic acid (γ-PGA) (1, 2, 3, and 4 %) to see which could outperform conventional cryoprotectant mixture (4 % sorbitol + 4 % sucrose) on cooked crayfish properties, such as physicochemical, textural qualities, oxidation reaction, water distributions, and microstructure integrity, during different freeze-thaw cycles. Crayfish quality characteristics improved significantly as γ-PGA concentration increased compared to control samples.Adding γ-PGA 4 % reduced the carbonyl content from 4.20 to 3.00 nmol/ mg protein during fluctuation-1 (F1), and from 4.15 to 2.80 nmol/ mg protein during fluctuation-2 (F2) compared to control samples. Furthermore, it increased the total sulfhydryl content from 4.15 and 4.76 to 6.19 and 6.47 mol/105 g protein during F1 and F2 and after five freeze-thaw cycles (FTC). This suggests that this concentration was more effective at controlling protein changes than other concentrations. γ-PGA generally enhanced the water-holding capacity by preventing protein denaturation and limiting ice crystal recrystallization. As a result, microstructure stability was evident, texture degradation was avoided, and the crayfish's color was preserved.


Subject(s)
Astacoidea , Polyglutamic Acid/analogs & derivatives , Water , Animals , Temperature , Freezing , Water/chemistry
4.
Food Chem X ; 20: 100953, 2023 Dec 30.
Article in English | MEDLINE | ID: mdl-37929267

ABSTRACT

Chinese cherry is an economically important fruit crop native to China. Flavor quality is greatly influenced by compositions of soluble sugars and organic acids. To better understand the flavor quality of Chinese cherry, we determined sugar and acid components in thirty-eight landrace and cultivar collections, and two wild resources using the HPLC method. Glucose and fructose were the main components, accounting for 85.91% of soluble sugars. Malic acid was the predominant organic acid, with an average proportion of 65.73% of total acids. Correlation and PCA analysis revealed seven key indicators for evaluating fruit flavor. Compared with wild Chinese cherry, the cultivated collections exhibited higher levels of soluble sugars, especially fructose, and lower levels of organic acid, particularly malic acid in fruits. Finally, we have established grading criteria for seven flavor indicators in Chinese cherry. Our study provides valuable references for identifying flavor compounds and improving flavor quality of Chinese cherry.

5.
Int J Biol Macromol ; 239: 124215, 2023 Jun 01.
Article in English | MEDLINE | ID: mdl-36996962

ABSTRACT

The goal of this study was to develop new biocomposite films that can better protect and prolong the shelf life of food. Here, a ZnO: eugenol@yam starch/microcrystalline cellulose (ZnO:Eu@SC) antibacterial active film was constructed. Because of the advantages of metal oxides and plant essential oils, codoping with these can effectively improve the physicochemical and functional properties of composite films. The addition of an appropriate amount of nano-ZnO improved the compactness and thermostability, reduced the moisture sensitivity, and enhanced the mechanical and barrier properties of the film. ZnO:Eu@SC exhibited good controlled release of nano-ZnO and Eu in food simulants. Nano-ZnO and Eu release was controlled by two mechanisms: diffusion (primary) and swelling (secondary). After loading Eu, the antimicrobial activity of ZnO:Eu@SC was significantly enhanced, resulting in a synergistic antibacterial effect. Z4:Eu@SC film extended the pork shelf life by 100 % (25 °C). In humus, the ZnO:Eu@SC film was effectively degraded into fragments. Therefore, the ZnO:Eu@SC film has excellent potential in food active packaging.


Subject(s)
Dioscorea , Eugenol , Eugenol/pharmacology , Starch , Anti-Bacterial Agents/pharmacology , Anti-Bacterial Agents/chemistry , Food Packaging
6.
Food Chem X ; 12: 100161, 2021 Dec 30.
Article in English | MEDLINE | ID: mdl-34877526

ABSTRACT

The proximal composition, amino acid, carbohydrate, and volatile profiles of caferana (Bunchosia glandulifera) seeds flour were here assessed. Seeds were also subjected to the following extraction processes: one with pressurized ethanol (PLE) and two with ethanol + supercritical CO2 mixture at different temperatures and pressures (SC1 and SC2). Extracts were characterized in terms of caffeine, total phenolic, and δ-lactam. The characterization of caferana seed and its extracts is unprecedented in terms of carbohydrate and volatiles profiles, besides the δ-lactam identification/isolation. SC2 extract exhibited a higher caffeine (9.3 mg/g) and δ-lactam (29.4 mg/g) content, whereas the PLE extract contained a higher total phenolic amount (3.0 mgGAE/g). Caferana is regionally associated to protective effects on mental health. Its byproduct (seed) revealed to be a promising source of bioactive compounds, and a potential raw material of nutritive extracts and flours that can be incorporated into pharmaceutical, nutraceutical, cosmetic, and food products.

7.
Int J Pharm ; 578: 119186, 2020 Mar 30.
Article in English | MEDLINE | ID: mdl-32112931

ABSTRACT

Finite dose experiments represent clinical use wherein depletion of dose, evaporation of excipients, and gradual change in vehicle composition may occur. In the present study, we attempted a mathematical approach for predicting skin permeation and concentration of a cosmetic active, rhododendrol (RD), from complex vehicle-based formulations applied in finite dose. In vitro skin permeation and concentration studies of RD were conducted from formulations containing water and polyols with concentrations ranging from 10 to 100% under infinite and finite dose conditions using vertical Franz diffusion cells. Observed data for skin permeation and the viable epidermis and dermis (VED) concentration of RD were estimated by the differential equations under Fick's second law of diffusion together with water evaporation kinetics and changes in the partition coefficient from vehicles to the stratum corneum. As a result, a goodness-of-fit was observed allowing accurate estimation of skin permeation and VED concentration of RD. This mathematical approach could become a useful tool to estimate the skin permeation and concentration of actives from topical formulation applied in finite dose conditions likened in actual use.


Subject(s)
Butanols/metabolism , Cosmetics/metabolism , Dermis/metabolism , Epidermis/metabolism , Administration, Cutaneous , Animals , Chemistry, Pharmaceutical/methods , Diffusion/drug effects , Kinetics , Permeability , Polymers/metabolism , Skin Absorption/physiology , Swine , Water/metabolism
8.
Food Chem ; 310: 125831, 2020 Apr 25.
Article in English | MEDLINE | ID: mdl-31787391

ABSTRACT

Two sets of nine ciders were made by cryo-extraction for two consecutive harvests combining three types of ice cider apple juices (mono-varietal, bi-varietal and multi-varietal) and three autochthonous Saccharomyces bayanus yeast strains. The type of juice significantly influenced the pH values and the contents of sorbitol and shikimic acid in the ice juices. The strains used as starters did develop the fermentation producing ciders with alcoholic degrees between 8.75 and 11.52 (% v/v) and volatile acidities lower than 0.55 g acetic acid/L. Regarding the ice ciders, the apple mixture significantly influenced the levels of methanol (higher in mono-varietal ciders), 2-phenylethanol, and some minor acetate esters (higher in the bi-varietal ciders). The last ciders were also more floral, buttery, acidic and bitter than those made from mono- and multi-varietal juices. In the first harvest, the ciders obtained from the bi-varietal apple mixture scored lower for overall sensory quality.


Subject(s)
Alcoholic Beverages , Malus , Saccharomyces/metabolism , Acetic Acid/metabolism , Alcoholic Beverages/analysis , Chemical Fractionation/methods , Fermentation , Freezing , Humans , Malus/chemistry , Taste , Volatile Organic Compounds/analysis
9.
Food Chem ; 274: 376-383, 2019 Feb 15.
Article in English | MEDLINE | ID: mdl-30372954

ABSTRACT

Ice cider is a special product made from apple juices enriched by freezing. In this paper, the method of obtaining the ice juices (cryo-extraction and exhaustion) and the year of harvest have been evaluated. For this purpose, a controlled raw apple mixture and an autochthonous Saccharomyces bayanus strain were used throughout the study. Both the enrichment system and the year of harvest significantly influenced the levels of total phenols, sucrose, malic acid, ethyl acetate and 2-phenylethanol. The ciders made by cryo-extraction presented the higher sugar/acidity and sugar/polyphenol ratios. These ciders were more fruity, less astringent and scored better for quality than those obtained by exhaustion. Additionally, a preliminary assay of juice enrichment by cryo-concentration is described. The corresponding ciders presented higher methanol and lower 2-phenylethanol contents than those obtained by the cryo-extraction and exhaustion methods.


Subject(s)
Food Handling/methods , Freezing , Fruit and Vegetable Juices/analysis , Ice , Malus/chemistry , Taste , Malus/metabolism , Malus/microbiology , Polyphenols/analysis , Saccharomyces/metabolism , Sugars/analysis
10.
Int J Pharm ; 534(1-2): 60-70, 2017 Dec 20.
Article in English | MEDLINE | ID: mdl-29024788

ABSTRACT

Oral vaccines present an attractive alternative to injectable vaccines for enteric diseases due to ease of delivery and the induction of intestinal immunity at the site of infection. However, susceptibility to gastrointestinal proteolysis, limited transepithelial uptake and a lack of clinically acceptable adjuvants present significant challenges. A further challenge to mass vaccination in developing countries is the very expensive requirement to maintain the cold chain. We recently described the effectiveness of a Single Multiple Pill® (SmPill®) adjuvanted capsule approach to enhance the effectiveness of a candidate enterotoxigenic Escherichia coli (ETEC) oral vaccine. Here it was demonstrated that this delivery system maintains the antigenicity of ETEC colonisation factor antigen I (CFA/I) and the immunostimulatory activity of the orally active α-Galactosylceramide (α-GalCer) adjuvant after storage of SmPill® minispheres under room temperature and extreme storage conditions for several months. In addition, the internal structure of the cores of SmPill® minispheres and antigen release features at intestinal pH were found to be preserved under all these conditions. However, changes in the surface morphology of SmPill® minispheres leading to the antigen release at gastric pH were observed after a few weeks of storage under extreme conditions. Those modifications were prevented by the introduction of an Opadry® White film coating layer between the core of SmPill® minispheres and the enteric coating. Under these conditions, protection against antigen release at gastric pH was maintained even under high temperature and humidity conditions. These results support the potential of the SmPill® minisphere approach to maintain the stability of an adjuvanted whole cell killed oral vaccine formulation.


Subject(s)
Adjuvants, Immunologic/chemistry , Antigens/chemistry , Capsules/chemistry , Vaccines/chemistry , Administration, Oral , Animals , Capsules/pharmacology , Drug Delivery Systems/methods , Escherichia coli/drug effects , Fimbriae Proteins/metabolism , Galactosylceramides/metabolism , Hot Temperature , Humidity , Hydrogen-Ion Concentration , Male , Mice , Mice, Inbred C57BL , Vaccines/pharmacology
11.
J Chem Neuroanat ; 86: 19-34, 2017 Dec.
Article in English | MEDLINE | ID: mdl-28728966

ABSTRACT

CLARITY is a tissue clearing method, which enables immunostaining and imaging of large volumes for 3D-reconstruction. The method was initially time-consuming, expensive and relied on electrophoresis to remove lipids to make the tissue transparent. Since then several improvements and simplifications have emerged, such as passive clearing (PACT) and methods to improve tissue staining. Here, we review advances and compare current applications with the aim of highlighting needed improvements as well as aiding selection of the specific protocol for use in future investigations.


Subject(s)
Imaging, Three-Dimensional/methods , Immunohistochemistry/methods , Tissue Fixation/methods , Animals , Coloring Agents , Humans
12.
Int J Pharm ; 530(1-2): 165-172, 2017 Sep 15.
Article in English | MEDLINE | ID: mdl-28754511

ABSTRACT

pH shift-induced aggregation is frequently observed in downstream processing of monoclonal antibodies and has been shown to depend on solvent composition. To quantify the stabilizing effect of polyol additives against aggregation, we determined aggregation rate constants in the presence of a set of 14 compounds. Rate constants were then correlated with molecular descriptors in a quantitative structure activity relationship (QSAR) approach. The molecular size, volume, the charge, number of hydrogen acceptors, the stereochemistry and hydrophobicity of the compounds were identified as important descriptors. Generally larger compounds with a balanced surface polarity tend to inhibit aggregation better while hydrophobicity plays an important role at the nucleation phase, with hydrophobic compounds being more potent at inhibiting aggregation.


Subject(s)
Antibodies, Monoclonal/chemistry , Polymers/chemistry , Hydrogen-Ion Concentration , Hydrophobic and Hydrophilic Interactions , Quantitative Structure-Activity Relationship , Solvents
13.
Eur J Pharm Sci ; 108: 50-61, 2017 Oct 15.
Article in English | MEDLINE | ID: mdl-27586019

ABSTRACT

Aim of present work was to apply quality by design (QbD) principles for the development of proliposome of poorly soluble lopinavir (LPV). The patient-centric quality target product profile (QTPP) was defined and critical quality attributes (CQAs) earmarked. Risk assessment studies were carried out to identify the probable risks affecting the CQAs of the product. On the basis of preliminary study, lipid:drug ratio and amount of carrier were selected as critical material attributes (CMAs) and were optimized by face centered central composite design. Liposome vesicle size, drug entrapment efficiency and % drug release after 60min were selected as CQAs and mathematical relationship between CQAs and CMAs was derived using multiple linear regression analysis. Optimum composition of CMAs, identified using numerical optimization and desirability function, demonstrated excellent entrapment efficiency (>90%), drug release characteristics (>95% in 60min) and had vesicle size of 659.7±23.1nm. Solid state characterization studies (Differential Scanning Calorimetry, scanning electron microscopy and X-ray diffraction) were performed for optimized proliposome, suggested transformation of crystalline to amorphous form. Oral bioavailability study in Wistar rats revealed that LPV proliposome exhibited 2.24 and 1.16 fold higher bioavailability than pure LPV and available commercial formulation of LPV/RTV (lopinavir+ritonavir), respectively. Stability study of the optimized LPV loaded proliposome was performed as per ICH guideline and was found to be stable for period of 6months. Overall results of the study indicate that the proliposome offers advantages of enhanced oral bioavailability for poorly soluble LPV.


Subject(s)
Anti-Retroviral Agents/administration & dosage , Liposomes/chemistry , Lopinavir/administration & dosage , Nanoparticles/chemistry , Administration, Oral , Animals , Anti-Retroviral Agents/chemistry , Anti-Retroviral Agents/pharmacokinetics , Biological Availability , Chemistry, Pharmaceutical , Drug Combinations , Drug Delivery Systems , Drug Liberation , Drug Stability , Female , Humans , Lopinavir/chemistry , Lopinavir/pharmacokinetics , Particle Size , Rats, Wistar , Ritonavir/administration & dosage , Ritonavir/chemistry , Solubility
14.
J Control Release ; 233: 162-73, 2016 07 10.
Article in English | MEDLINE | ID: mdl-27157995

ABSTRACT

Diarrhoeal infections are a major cause of morbidity and mortality with enterotoxigenic Escherichia coli (ETEC) and cholera imposing a significant global burden. There is currently no licensed vaccine for ETEC. Development of new nonliving oral vaccines has proven difficult due to the physicochemical and immunological challenges associated with the oral route. This demands innovative delivery solutions to protect antigens, control their release and build in immune-stimulatory activity. We describe the Single Multiple Pill® (SmPill®) vaccine formulation which combines the benefits of enteric polymer coating to protect against low gastric pH, a dispersed phase to control release and aid the solubility of non-polar components and an optimized combination of adjuvant and antigen to promote mucosal immunity. We demonstrate the effectiveness of this system with whole cell killed E. coli overexpressing colonization factor antigen I (CFA/I), JT-49. Alpha-galactosylceramide was identified as a potent adjuvant within SmPill® that enhanced the immunogenicity of JT-49. The bacteria associated with the dispersed phase were retained within the capsules at gastric pH but released at intestinal pH. Vaccination with an optimized SmPill® formulation promoted CFA/I-specific immunoglobulin A (IgA) responses in the intestinal mucosa in addition to serum IgG and a solubilized adjuvant was indispensable for efficacy.


Subject(s)
Adjuvants, Immunologic/administration & dosage , Antigens, Bacterial/immunology , Escherichia coli Vaccines/administration & dosage , Fimbriae Proteins/immunology , Galactosylceramides/administration & dosage , Administration, Oral , Animals , Antibodies, Bacterial/blood , Antibodies, Bacterial/immunology , Capsules , Diarrhea/prevention & control , Escherichia coli/immunology , Escherichia coli Infections/prevention & control , Female , Immunoglobulin A/immunology , Immunoglobulin G/blood , Immunoglobulin G/immunology , Intestines/immunology , Mice, Inbred BALB C , Vaccination/methods
15.
Int J Pharm ; 496(2): 850-62, 2015 Dec 30.
Article in English | MEDLINE | ID: mdl-26474964

ABSTRACT

The purpose of this work was to evaluate the influence of the co-encapsulation of lyoprotectants with insulin into PLGA nanoparticles, on the stability of the protein and nanoparticles upon lyophilization. Different lyoprotectants were used, namely trehalose, glucose, sucrose, fructose and sorbitol at 10% (w/v). Insulin-loaded PLGA nanoparticles with co-encapsulated lyoprotectants achieved a mean particle size of 386-466nm, and a zeta potential ranging between -34 and -38mV, dependent on the lyoprotectant used. Formulations had association efficiencies and loading capacities of 85-91% and 10-12%, respectively. The lyophilization process increased the colloidal stability of nanoparticles, and maintained their spherical shape and smooth surface, particularly in presence of lyoprotectants. XRPD revealed that the lyophilizates of nanoparticles with co-encapsulated lyoprotectants were amorphous, whereas formulations with externally added lyoprotectants, except trehalose, showed crystallinity. FTIR assessment showed that co-encapsulating lyoprotectants better preserved insulin structure upon lyophilization with a spectral area overlap of 82-87%, compared to only 72% in lyoprotectant absence. These results were confirmed by circular dichroism spectroscopy. Surprisingly, the simultaneous co-encapsulation and addition of lyoprotectants was detrimental to protein stabilization. The insulin in vitro release studies demonstrated that formulations with co-encapsulated trehalose, glucose, sucrose, fructose and sorbitol achieved 83%, 69%, 70%, 77% and 74%, respectively after 48h. In contrast, formulations added with those lyoprotectants prior lyophilization showed a lower release rate not higher than 60% after 48h. This work gives rise to a different promising strategy of co-encapsulating lyoprotectants and therapeutic proteins, to better stabilize protein structure upon lyophilization.


Subject(s)
Lactic Acid/chemistry , Nanoparticles/chemistry , Polyglycolic Acid/chemistry , Circular Dichroism , Drug Stability , Freeze Drying , Particle Size , Polylactic Acid-Polyglycolic Acid Copolymer , Protein Structure, Secondary , Solubility , X-Ray Diffraction
16.
Food Chem ; 187: 189-96, 2015 Nov 15.
Article in English | MEDLINE | ID: mdl-25977015

ABSTRACT

The goal of this work was to characterize how the date of harvest of 'Viking' aronia berry impacts juice pigmentation, sugars, and antioxidant activity. Aronia juice anthocyanins doubled at the fifth week of the harvest, and then decreased. Juice hydroxycinnamic acids decreased 33% from the first week, while proanthocyanidins increased 64%. Juice fructose and glucose plateaued at the fourth week, but sorbitol increased 40% to the seventh harvest week. Aronia juice pigment density increased due to anthocyanin concentration, and polyphenol copigmentation did not significantly affect juice pigmentation. Anthocyanin stability at pH 4.5 was similar between weeks. However, addition of quercetin, sorbitol, and chlorogenic acid to aronia anthocyanins inhibited pH-induced loss of color. Sorbitol and citric acid may be partially responsible for weekly variation in antioxidant activity, as addition of these agents inhibited DPPH scavenging 13-30%. Thus, aronia polyphenol and non-polyphenol components contribute to its colorant and antioxidant functionality.


Subject(s)
Anthocyanins/chemistry , Antioxidants/analysis , Beverages/analysis , Carbohydrates/analysis , Photinia/chemistry , Plant Extracts/chemistry , Polyphenols/analysis , Fruit/chemistry , Fruit/growth & development , Photinia/growth & development , Proanthocyanidins/analysis
17.
Carbohydr Polym ; 113: 225-30, 2014 Nov 26.
Article in English | MEDLINE | ID: mdl-25256479

ABSTRACT

Microwave irradiation is a rapid and efficient method to synthesize oligomers and can be employed in polysaccharides production. As an artificial polysaccharide, polydextrose is known for its solid performance in food processing and its additional health benefits. This study was aimed at producing polydextrose by microwave irradiation using glucose and sorbitol as substrates; water and phosphoric acid as initiator and catalyst. The actual maximum yield was 99%. Synthetic polydextrose were purified by ethanol elution and Sepherdex G-25 column chromatography. Its purity was demonstrated by the high-performance gel-permeation chromatography as a single symmetrical sharp peak, additionally the average molecular weight was calculated to be 2.131 kDa. FT-IR spectra showed that the synthesized polydextrose has the structural feature similar to Polydextrose-Litesse(®). In vitro fermentation revealed that polydextrose possesses the biological function similar to Polydextrose-Litesse(®) in increasing the concentration of short chain fatty acid and decreasing pH. This research demonstrated the feasibility of a rapid and efficient microwave mediated method to synthesize polydextrose and potentially other value added carbohydrate polymers.


Subject(s)
Glucans/analysis , Glucans/chemical synthesis , Microwaves , Glucans/physiology
18.
Int J Pharm ; 456(2): 370-81, 2013 Nov 18.
Article in English | MEDLINE | ID: mdl-24036086

ABSTRACT

This study aims to monitor the secondary structure behaviour of insulin when it is encapsulated into solid lipid nanoparticles (SLN), under the influence of several critical processing parameters. Insulin was used as a therapeutic protein model. Physicochemical properties of insulin-loaded SLN (Ins-SLN) were assessed, with special focus on the insulin secondary structure after its encapsulation into SLN and after freeze-drying using different cryoprotectants (glucose, fructose and sorbitol). Additionally, a 6-month stability study was performed to evaluate the maintenance of insulin secondary structure over time at different storage conditions (4 °C/60% RH, 25 °C/60% RH, 40 °C/75% RH). Ins-SLN were successfully produced with a mean and narrow particle size around 400 nm, zeta potential around -13 mV, an insulin association efficiency of 84%. Physical-chemical properties of SLN were maintained after freeze-drying. FTIR results showed that encapsulated insulin maintained a native-like structure in a degree of similarity around 92% after production, and 84% after freeze-drying. After 6 months, freeze-dried Ins-SLN without cryoprotectant stored at 40 °C/75% RH presented the same degree of structure preservation and morphology. Results revealed that insulin structure can be significantly protected by SLN matrix itself, without a cryoprotectant agent, even using a non-optimized freeze-drying process, and under the harsher storage conditions. Multivariable experimental settled the process parameters to fit with the desired product quality attributes regarding protein and nanoparticle stability.


Subject(s)
Cryoprotective Agents/chemistry , Freeze Drying/methods , Insulin/chemistry , Lipids/chemistry , Nanoparticles/chemistry , Drug Stability , Drug Storage/methods , Humans , Particle Size
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