Este archivo ha sido creado el 10-1-2024 por Mª Carmen Alfaro Rodríguez GENERAL INFORMATION ------------------ 1. Dataset title: Dataset utilizados para la preparación del artículo Effect of a Change in the CaCl2/Pectin Mass Ratio on the Particle Size, Rheology and Physical Stability of Lemon Essential Oil/W Emulgels 2. Authorship: Name:José Muñoz Institution: Universidad de Sevilla Email:jmunoz@us.es ORCID:0000-0002-1709-722X Name:Paula Prieto Institution: Universidad de Sevilla Email:paulaprietovargas@gmail.com ORCID: Name:Mª Carmen Garcia Institution: Universidad de Sevilla Email:mcgarcia@us.es ORCID: 0000-0001-9490-3937 Name:Mª Carmen Alfaro Institution: Universidad de Sevilla Email:alfaro@us.es ORCID:0000-0002-0110-2290 DESCRIPTION ---------- 1. Dataset language: Inglés 2. Abstract: A three-step (rotor-stator-microfluidization-rotor stator) protocol was used to prepare 15% lemon essential oil in water emulgels using a mixture of Tween 80 and Span 20 surfactants as low molecular mass emulsifiers and 0.4% low-methoxyl citrus peel pectin as a gelling agent. Ca2+ was used as a gel-promoting agent. Different CaCl2/pectin mass ratio values from 0.3 to 0.7 were used. Emulgels showed a microstructure consisting of oil droplets embedded in a sheared gel matrix, as demonstrated by bright field optical microscopy. Laser diffraction tests showed multimodal particle size distributions due to the coexistence of oil droplets and gel-like particles. Multiple light scattering tests revealed that the physical stability of emulgels was longer as the CaCl2/pectin mass ratio decreased and that different destabilization mechanisms took place. Thus, incipient syneresis became more important with increasing CaCl2 concentration, but a parallel creaming mechanism was detected for CaCl2/pectin mass ratio values above 0.5. Dynamic viscoelastic and steady shear flow properties of the emulgels with the lowest and highest CaCl2/pectin mass ratio values were compared as a function of aging time. The lowest ratio yielded an emulgel with enhanced connectivity among fluid units as indicated by its wider linear viscoelastic region, higher storage modulus, loss modulus and viscosity values, and more shear thinning properties than those of the emulgel formulated with the highest CaCl2/pectin mass ratio. The evolution of the dynamic viscoelastic properties with aging time was consistent with the information provided by monitoring scans of backscattering as a function of sample height 3. Keywords: Emulgel; pectina de cáscaras de cítrico de bajo metoxilo; aceite esencial de limón; gel cizallado; reología; estabilidad física. Emulgel; low-methoxyl citrus peel pectin; lemon essential oil; sheared gel; rheology; physical stability 4. Date of data collection:3-10-2022 hasta 25-11-2022 5. Publication Date: 6. Grant information: Grant Agency:FEDER/Consejería de Transformación Económica, Industria, Conocimiento, y Universidades de la Junta de Andalucía (Programa Operativo FEDER 2014-2020) Grant Number: Proyecto US-1380760 ACCESS INFORMATION ------------------------ 1. Creative Commons License of the dataset: CC BY-NC-ND 2. Dataset DOI: https://doi.org/10.12795/11441/153617 3. Related publication: Muñoz, J., Prieto-Vargas, P., García, M. C., & Alfaro-Rodríguez, M. C. (2023). Effect of a Change in the CaCl2/Pectin Mass Ratio on the Particle Size, Rheology and Physical Stability of Lemon Essential Oil/W Emulgels. Foods, 12(6), 1137. DOI:10.3390/foods12061137 VERSIONING AND PROVENANCE --------------- 1. Last modification date: 2. Were data derived from another source?: No METHODOLOGICAL INFORMATION ----------------------- 1. Description of the methods used to collect and generate the data: 1. Materials Emulgels were formulated using lemon essential oil purchased from Bidah-Chaumel (Spain), Tween 80 (HLB 15) and Span 20 (HLB 8.6), both from Sigma Aldrich (Spain), low-methoxyl citrus pectin (Aglupectin LC S18YP, methoxylation degree: 37–41%), kindly supplied by JRS Silvateam Ingredients Srl (Italy), citrate buffer solution containing deionized water, citric acid and tris-sodium citrate 2-hydrate at pH = 4.2, both reagents supplied by Panreac (Spain), calcium chloride dehydrate provided by Sigma-Aldrich (Spain) and, deionized water. The emulgels studied contained 15 wt% lemon essential oil, 15 wt% of a mixture of Tween 80 and Span 20, (Tween 80/Span 20) mass ratio: 1.13 which results in an HLB number of 12, which had previously been optimized. The present study was carried out with a fixed pectin concentration (0.4 wt%) and a variable CaCl2/pectin mass ratio (R) which ranged from 0.3 to 0.7. These values were previously selected to obtain samples which looked homogeneous by visual observation. Concerning the protocol of emulgel preparation, firstly, a coarse emulsion (batches of 200 g) was prepared, at room temperature, using a rotor-stator Ultra-Turrax T50 homogenizer with the S50-G45F dispersion unit. The aqueous phase was prepared by adding the appropriate amount of deionized water, emulsifiers (Tween 80 and Span 20), citrate buffer solution (pH = 4), and pectin while stirring for 3600 s at 2000 rpm. Afterwards, the lemon essential oil was gradually added to the aqueous phase stirring at 2000 rpm for 40 s, and subsequently, the same device was used for 90 additional seconds at 4000 rpm. Subsequently, finer emulsions were obtained using a microfluidizer M-110P (Microfluidics, EEUU) with chambers F12Y and H30Z arranged in series, after two passes at 137.9 MPa. Finally, emulgels were obtained by adding CaCl2 in the form of a solution (7% w/v stock solution) and stirring at 8000 rpm for 30 s in the Ultra-Turrax T50 homogenizer. This final mechanical treatment followed the method reported by Lupi et al. (2015) [31] and Lorenzo et al. (2013) [7]. Once prepared, the emulgels were left to rest in an oven at 25 °C until characterization. In Table 1 the composition of the emulgels is shown. The RX nomenclature will be used to denote the emulgels, with X being the CaCl2/pectin mass ratio; e.g., R0.3 standing for an emulgel formulated with a CaCl2/pectin mass ratio of 0.3. Table 1. Composition of the emulgels studied. RX stands for the CaCl2/pectin mass ratio. wt% R0.3 R0.4 R0.5 R0.6 R0.7 Pectin 0.4 0.4 0.4 0.4 0.4 CaCl2 0.12 0.16 0.20 0.24 0.28 Tween 80 7.95 7.95 7.95 7.95 7.95 Span 20 7.05 7.05 7.05 7.05 7.05 Lemon Oil 15 15 15 15 15 Water 69.48 69.44 69.40 69.36 69.32 2. Sample Characterization 2.1. Particle Size Distribution The particle size distribution (PSD) of samples was obtained using a Malvern Mastersizer 2000 laser diffraction device. The indexes of refraction for lemon essential oil and water were 1.474 and 1.330, respectively and the absorption index was 0.001. Each test was performed at room temperature and in duplicate. 2.2. Multiple Light Scattering The physical stability of all the samples studied was characterized by Turbiscan Lab-Expert equipment (Formulation, France) based on the principle of multiple light scattering. The analyzer is equipped with a pulsed near-infrared light source (λ = 880 nm) and synchronous optical detectors that determine the intensity of the backscattered light. In opaque samples, the backscattering profiles are analyzed rather than the transmitted light profiles. Changes in the backscattering profiles, as a function of measuring cell height, can be used to detect and characterize physical instabilities. Thus, local variations of the profiles at the top or bottom of the sample are the consequence of particle migration, whereas global variations along the whole height of the sample are the result of particle size variations. 2.3. Rheological Characterization Small-amplitude oscillatory tests and flow curves were performed using a Haake Mars II controlled stress rheometer (Thermo-Scientific, Karlsruhe, Germany), with a serrated plate-plate geometry, PP60R (diameter: 60 mm and gap: 1 mm). The equilibration time before the rheological measurement was 300 s and the temperature was fixed at 20 °C. A stress sweep from 0.1 to 20 Pa was carried out at a frequency of 1 Hz to estimate the linear viscoelastic range. Subsequently, mechanical spectra were obtained from 0.008 to 10 Hz at a shear stress amplitude within the linear viscoelastic zone. Flow curves were run using a controlled stress protocol from 0.1 to 10 Pa. All measurements were made in duplicate with fresh samples. The flow curves were fitted to the power-law equation: ηa = K·γ ̇ (n−1) (1)where ηa is the apparent viscosity (Pa·s), γ ̇ the shear rate (s−1), K is the consistency index (Pa·sn), and n is the so-called “power-law flow index”. 2.4. Optical Microscopy Emulgels were observed using an optical microscope, Axio Scope A1 (Carl Zeiss). Samples were observed at room temperature, using 100× oil immersion objective using the bright field technique. 2.2.5. Statistical Analysis The standard deviation of the mean of replicates was calculated to determine the occurrence of significant differences among the results obtained. 2. Data processing methods: [Recomendado | Describir cómo se ha generado el conjunto de datos publicado a partir de los datos primarios recogidos.] Los datos originales obtenidos de los diferentes ensayos en los distintos equipos antes indicados se han exportado al programa Origin 8.0, se ha hecho el análisis estadístico y se han representado gráficamente los valores medios y sus desviaciones estándar. 3. Software or instruments needed to interpret the data: Microsoft Office 4. Information about instruments, calibration and standards: 5. Environmental or experimental conditions: Temperatura =20ºC 6. Quality-assurance procedures performed on the data: FILE OVERVIEW ---------------------- 1. Explain the file naming conversion, si es aplicable: Dataset of the manuscript published in Foods in 2023 whose doi is: DOI:10.3390/foods12061137 2. File list: File name:DatasetFoods-2023.docx Description: The following results are shown: a) the particle size distributions (mean and standard deviation) of emulgels and emulsions with a pectin/CaCl2 ratio of 0.3 and 0.7 at 1 day of aging, b) profiles of backscattered light in reference mode (DBS%) as a function of the height of the measurement cell and the time of aging (15 days) for emulgels with a pectin/CaCl2 ratio of 0.3 (R0.3); 0.4 (R0.4); 0.5 (R0.5); 0.6 (R0.6) and 0.7 (R0.7), c) parameter calculated from the backscattered light profiles, TSI, as a function of the aging time for the different emulgels studied (R0.3, R0.4, R0.5, R0.6 and R0.7), d) stress sweeps as a function of aging time for emulgels R0.3 and R0.7, e) frequency sweeps for emulgels R0.3 and R0.7 on day 1, 7 and 15 of storage. The mean values of G' and G" are presented as well as their standard deviation, f) flow curves (viscosity-shear rate) on day 1 and day 15 for the emulgels R0.3 and R0.7. The mean values and standard deviation are presented, as well as the fit of the experimental data to a potential equation. 3. Relationship between files: 4. File format: .docx 5. If the dataset includes multiple files, specify the directory structure and relationships between the files: SPECIFIC INFORMATION FOR TABULAR DATA ------------------------------------------- 1. Name file:DatasetFoods-2023 2. Number of rows and columns: 3. Variables list: Variable name: Description: Units of measure or value labels | Unidades de medida o etiquetas de valor: 4. Codes or symbols for missing data: Code or symbol:D Definition:particle diameter Code or symbol:Mean% Definition:The mean of the %Volume Code or symbol:SD Definition:standard deviation Code or symbol:f Definition:oscillation frequency in Hertzios Code or symbol:Mean G' Definition:The mean of storage modulus values Code or symbol:Mean G" Definition:The mean of loss modulus values Code or symbol:tau Definition:shear stress Code or symbol:ganma point Definition:shear rate Code or symbol:eta Definition:apparent viscosity Code or symbol:d1 Definition:1 day of aging Code or symbol:d15 Definition:15 days of aging Code or symbol:ganma point fit Definition:the shear rate that results the experimental data to potential-law model Code or symbol:TSI Definition:Turbiscan stability index 5. Special formats or abbreviations used: MORE INFORMATION --------------