The aim of this work was preparation and characterization of nanoemulsions containing Caprylic/Capric Triglyceride, Caprylic/Capric/Linoleic Triglyceride and Caprylic/Capric/Succinic Triglyceride as the oil phase. Stable emulsion system was obtained by using Polisorbate 40 as emulsifier and n-buthanol as cosurfactant. The formulations were prepared by phase inversion composition method (PIC), one of the low energy emulsification method, by stepwise water addition to the mixture of oil and surfactant, at room temperature(25oC).The mixture was stirred by using a magnetic stirrer. The type of the emulsions was confirmed by conductivity measurement. The particles size distribution was analyzed by Dynamic Light Scattering measurement technique using Zetasizer Nano ZS (Malvern Instruments, UK). Rheological studies of the systems were carried out using Brookfield Rheometer Model -R/SPlus. The obtained results showed that properties of the emulsions depend on kind of the oil phase. It was observed that the increase of oil phase polarity causes the increase of the particle size of internal phase

Jaworska, Małgorzata

Ogonowski, Jan

Sikora, Elżbieta

English

Periodica Polytechnica (Budapest University of Technology and Economics)

43The influence of glicerides oil phase on O/W nanoemulsion formation by pic method 2014 58 SupThe influence of glicerides  oil phase on O/W nanoemulsion  formation by pic method Małgorzata Jaworska / Elżbieta Sikora / Jan Ogonowskireceived 31 OctOber 2012; accepted 27 March 2013AbstractThe aim of this work was preparation and characterization of nanoemulsions containing Caprylic/Capric Triglyceride, Caprylic/Capric/Linoleic Triglyceride and Caprylic/Capric/Succinic Triglyceride as the oil phase. Stable emulsion system was obtained by using Polisorbate 40 as emulsifier and n-buth-anol as cosurfactant.The formulations were prepared by phase inversion com-position method (PIC), one of the low energy emulsification method, by stepwise water addition to the mixture of oil and surfactant, at room temperature(25oC).The mixture was stirred by using a magnetic stirrer. The type of the emulsions was con-firmed by conductivity measurement. The particles size distri-bution was analyzed by Dynamic Light Scattering measure-ment technique using Zetasizer Nano ZS (Malvern Instruments, UK). Rheological studies of the systems were carried out using Brookfield Rheometer Model -R/SPlus. The obtained results showed that properties of the emul-sions depend on kind of the oil phase. It was observed that the increase of oil phase polarity causes the increase of the particle size of internal phase. Keywordstriglycerides · nanoemulsion · PIC method1 IntroductionNanoemulsions are the novel class of emulsions with high degree of inert phase dispersion.Particles of nanoemulsions are too small to scatter visible light (droplet size are in the range between 20 - 200 nm), that makes them optically transparent or translucent. In contrast to microemulsions, nanoemulsions are characterized by kinetic stability [1-6]. As a form of cosmet-ics products they can relatively easily penetrate into the skin, exhibit a high degree of hydration and soften the skin and have a very good user properties (ease of spreading on the skin, no greasy feeling). An additional advantage of these emulsions type, as a form of cosmetic, is no inherent creaming, sedimen-tation, flocculation or coalescence usually have observed in case of macroemulsions.Triglycerides, are the popular cosmetic and pharmaceuti-cal ingredients. From chemical point of view they are esters of glycerin and fatty acids. They usually applied in skin care products as emollients, lipophilic vehicles, skin permeation enhancers and solubilisers. Their properties strongly depend on chemical composition [7,8,9]. The natural sources of triglycer-ides used as the cosmetic ingredients are vegetable oil. Also the synthetic esters including caprylic/ capric triglycerides (Fig. 1) are popular.Caprylic/capric triglycerides are fully saturated triglycer-ides, with excellent emolliency and good user properties, e.g. easy spreading orno occlusive feeling. It is entirely derived from vegetable resources and offers a stable alternative to mineral or vegetable oil. They are non-toxic and non-irritating   58(Sup), pp. 43-48, 2014DOI:10.3311/PPch.7299http://www.pp.bme.hu/ch/article/view/7299Creative Commons Attribution bresearch articleMałgorzata JaworskaFaculty of Chemical Engineering and Technology, Institute of Organic Chemistry and Technology, Cracow University of Technology, Warszawska 24, 31-155 Krakow, Poland e-mail: mjaworska@chemia.pk.edu.plEl bieta SikoraJan OgonowskiFaculty of Chemical Engineering and Technology, Institute of Organic Chemistry and Technology, Cracow University of Technology, Warszawska 24, 31-155 Krakow, Poland Fig. 1. Chemical structure – caprylic/capric triglyceride.P Periodica PolytechnicaChemical Engineering44 Per. Pol. Chem. Eng. Małgorzata Jaworska / Elżbieta Sikora / Jan Ogonowskito skin, often used as solvent and vehicle for vitamins and nutri-tional active [8]. They have very low reactivity with chemically sensitive pharmaceutical actives. They were selected as the oil phase in microemulsion O/W, used as the drug delivery system, to transport ketoprofen [10] and in nanoemusion O/W contain-ing lidocaine, [2] also as based emulsions for danazol [11].The aim of this work was preparation and characterization of nanoemulsions containing as the oil phase Caprylic/Capric Triglycerides, Caprylic/Capric/Linoleic Triglycerides and Caprylic/Capric/Succinic Triglycerides. The emulsions were stabilized by different type of Polisorbates. Stable emulsion system was  obtained by using Polisorbate 40 (PEG-20 Sorb-itan Palmitate) as emulsifier and n-buthanol as cosurfactant.2 Experimental2.1 MaterialsIn the studies, on the basis of elaborated formulation, stable emulsion were obtained. As an oil phase in the formulations, different kind of triglycerides have been applied (Table 1).Polisorbates 40, 60 and 80 were used as the emulsifiers. Additionally, the short-chain alcohols (ethanol, 1-propanol, buthanol) were tested as cosurfactants. The aqueous phase was distilled water. All ingredients used in the formulation are char-acterized in Table 2.2.2 Formation of O/W nanoemulsionsThe emulsions systems were prepared by phase inversion method (PIC) by stepwise water (W) addition to the mixture of oil (O) and surfactant (S) and co-surfactant (CoS), at room temperature (25°C). The mixture was stirred by using a mag-netic stirrer, IKAC-MAG H 7 equipped with speed control. The emulsification process parameters are shown in Table 3.2.3 Assessment of rheological propertiesRheological properties of the emulsifiers and the obtained emulsions were studied using Brookfield Rheometer Model R/S-plus, equipped with a cone-plate type measuring system (cone C75-1), at room temperature 25°C (298 K). The rheo-logical studies were carried out with variable viscosity shear rate in the range of values from 1 to1000 s-1.2.4. Measurement of droplet sizeThe average internal phase droplet size of the emulsions were measured by Dynamic Light Scattering (DLS) method, using Malvern Zetasizer Nano ZS apparatus , which measures particle size (range from 0.3nm to 10μm) by scattering pho-tons from a sample and determine the change in diffracted light intensity. Scattering angle was 1730.3 Result and discussion3.1 Composition of obtained formulationThe results of the first stage of the study are presented in Table 4. After many tests it turned out that the stable emulsion system with Miglyol 812 could be obtain only when as the sta-bilizers mixture of Polisorbate 40 and n- buthanol was used, and only in specific concentration area (S:CoS=1:1, S/CoS:O=90:10). Ingredient Chemical structure Caprylic/Capric  Triglyceride (M812)Caprylic/Capric/Linoleic Triglyceride (M818)Caprylic/Capric/Succinic  Triglyceride (M829)Caprylic Acid C7H15COOH (C8:0) 50.0 – 65.0 45 – 65 45 – 55Capric Acid C9H19COOH (C10:0) 30.0 – 45.0 30 – 45 30 – 40Linoleicacid C17H39COOH (C18:2) - 2 – 5 -Succinic Acid (CH2COOH)2 - - 15 – 20Trade name INCI name Characterization Name of suppliersTween 80® Polysorbate 80 PEG 20 Sorbitan Oleate emulsifier; HLB=15.0 Croda PolandTween 60® Polysorbate 60 PEG 20 Sorbitan Stearate emulsifier; HLB = 14.9 Croda PolandTween 40® Polysorbate 40 PEG 20 Sorbitan Palmitate emulsifier; HLB=15.6 Croda PolandMiglyol 812® Caprylic/Capric/Triglyceride emollient SasolMiglyol 818® Caprylic/Capric/SuccinicTriglyceride emollient SasolMiglyol 829® Caprylic/Capric/LinoleicTriglyceride emollient Sasolethanol - cosurfactant POCh1-propanol - cosurfactant POChbuthanol - cosurfactant POChTab. 2. Components used in the studies.Tab. 1. Composition of fatty acids [9].45The influence of glicerides oil phase on O/W nanoemulsion formation by pic method 2014 58 SupIn the next step of studies different type of triglycerides were used as an oil phase (Table 5).From the results shown in table 5 it could be concluded that only emulsions containing Miglyol 829 weren’t stable. It means that stability of formulation depend on kind of the used triglycerides. It probably caused by differences in polarity of the oils. When more polar oil had been used in formulation the less stable emulsions were obtained.3.2 Characterization of the stable emulsionsThe data presented in table 6 and on the figure 2 show that the stable, transparent, o/w nanoemulsion, containing as an oil phase Miglyol 812 and Miglyol 818, could be obtained using Polisorbate 40 as the emulsifier and n-buthanol as cosurfactant.Tab. 3. Emulsification process parameters.Fig. 2. Macroscopic picture of composition NE5M812.Tab. 5. Formulations stabilized by Polisorbat 40 and n-buthanol.Legend: NE3M812 – emulsion w 3% content of Miglyol 812, NE5M812 – emulsion w 5% content of Miglyol 812,NE8M812– emulsion w 8% content of Miglyol812, NE3M818 – emulsion w 3% content of Miglyol 818, NE5M818 – emulsion w 5% content of Miglyol 818,NE8M818– emulsion w 8% content of Miglyol 818, NE3M829 – emulsion w 3% content of Miglyol 829, NE5M829 – emulsion w 5% content of Miglyol 829,NE8M829– emulsion w 8% content of Miglyol 829.IngredientComposition [% mas]NET80E NET80P NET80B NET60E NET60P NET60B NET40E NET40P NET40BMiglyol 812 5 5 5 5 5 5 5 5 5Aqua 45 45 45 45 45 45 45 45 45Polisorbate 80 25 25 25 - - - - - -Polisorbate 60 - - - 25 25 25 - - -Polisorbate 40 - - - - - - 25 25 25Ethanol 25 - - 25 - - 25 - -1-propanol - 25 - - 25 - - 25 -buthanol - - 25 - - 25 - - 25Stability no no no no no no no no yesTab. 4. Formulations with Miglyol 812 as the oil phase.Legend: NET80E – emulsion stabilized by Polisorbate 80 and ethanol, NET80P  – emulsion stabilized by Polisorbate 80 and 1-propanol,NET80B – emulsion stabilized by Polisorbate 80 and buthanol, NET60E – emulsion stabilized by Polisorbate 60 and ethanol,NET60P  – emulsion stabilized by Polisorbate 60 and 1-propanol, NET60B – emulsion stabilized by Polisorbate 60 and buthanol,NET40E – emulsion stabilized by Polisorbate 40 and ethanol, NET40P  – emulsion stabilized by Polisorbate 40 and 1-propanol,NET40B – emulsion stabilized by Polisorbate 40 and buthanol.IngredientComposition [% mas]NE3M812 NE5M812 NE8M812 NE3M818 NE5M818 NE8M818 NE3M829 NE5M829 NE8M829Aqua 45 45 45 45 45 45 45 45 45Polisorbate 40 26 25 23.5 26 25 23.5 26 25 23.5n-buthanol 26 25 23.5 26 25 23.5 26 25 23.5M812 3 5 8 - - - - - -M818 - - - 3 5 8 - - -M829 - - - - - - 3 5 8S/CoS:O 95:5 90:10 85:15 95:5 90:10 85:15 95:5 90:10 85:15Stability yes yes yes yes yes yes no no noParameter ValueEmulsification time 20 min.Emulsification temperature 25°CStirrer speed 300 rpmMethod of phase connection drop by dropPhase inversion composition (PIC) W→O/S/CoS46 Per. Pol. Chem. Eng. Małgorzata Jaworska / Elżbieta Sikora / Jan OgonowskiIt should be noticed that the concentration of oil phase influ-ences on internal phase droplets size. The emulsion NE8M812, which contains highest concentration (8%) of Miglyol 818 is characterized bythe smallest droplets size of the dispersed phase. Moreover, the obtained results showed that the ratio of oil phase to the surfactant mixture affects th properties of prepared emulsions.On the other hand , it was observed that there is no significant dif-ference between particle size of emulsions based on Miglyol 812 and Miglyol 818 with the same concentration of internal phase. Figures 3 – 5 show the comparison of particle size distribution between  nanoemulsions based on Miglyol 812 and Miglyol 818 with different oil phase concentration.3.3 Stability of nanoemulsionsThe samples were stored, at ambient temperature, for 24 hours, 47 hours, one week and one month. During the time Formulations Type of emulsion pH Appearance Surface tension[mN/m]Average droplet size [nm]PDINE3M812 O/W 6.00 transparent 25.16 242.5 0.039NE5M812 O/W 6.02 transparent 25.33 170.5 0.054NE8M812 O/W 5.85 transparent 25.25 115.9 0.156NE3M818 O/W 6.03 transparent 26.18 264.1 0.117NE5M818 O/W 6.07 transparent 26.43 123.5 0.087NE8M818 O/W 5.97 transparent 26.35 124.9 0.106Tab. 6. Properties of the stable emulsion systems.Fig. 3. Comparison of particle size distribution of nanoemulsion NE3M812 and NE3M818 with 3% of oil phase.Fig. 4. Comparison of particle size distribution of nanoemulsion NE5M812 and NE5M818 with 5% of oil phase.47The influence of glicerides oil phase on O/W nanoemulsion formation by pic method 2014 58 Supthe stability of the formulations were assessed visually. The emulsions were transparent and stable. The phase separation and degradation were not observed during these 2 months. All nanoemulsions showed no change in clarity and phase behavior.3.4 Rheological characterizationFigure 6 and 7 show that all nanoemulsions based on Mig-lyol 812 and Miglyol 818 are characterized by pseudoplastic behaviour. It is worth noting that the emulsions NE8M812 and NE8M818 with highest amount of oil phase are characterized by the highest viscosity. Moreover as  figure 8 shown there was no significant effect of the oil phase type on the rheological properties of obtained formulations.4 ConclusionsThe obtained results showed that properties of the emul-sions depend on kind of the oil phase. Stable emulsion sys-tems were prepared based on Miglyol 812 and 818 and sta-bilized by Polisorbat 40 as emulsifier and n-buthanol as cosurfactant. It may indicate that if the more polar oil base have been used (Miglyol 829) the less stable emulsion were obtained. Moreover, there was no significant effect of the oil base on the rheological properties of the obtained formulations. All nanoemulsions are non-Newtonian liquids with pseudo-plastic rheological behavior. Although, there are no signifi-cant differences in the physicochemical properties of nanoe-mulsions based on Miglyol 812 and Miglyol 818, however Miglyol 818 may be more efficient in the transport of active substances to the skin, due to the content of linolenic acid in its structure.Fig. 5. Comparison of particle size distribution of nanoemulsion NE8M812 and NE8M818 with 8% of oil phase.Fig. 8. Comparison of the viscosity of nanoemulsions based on Miglyol 812 and Miglyol 818, at shear rate γ = 100 s-1.Fig. 6. Comparison of the viscosity of nanoemulsions based on Miglyol 812, at 250°C.Fig. 7. Comparison of the viscosity of nanoemulsions based on Miglyol 818, at 250°C.48 Per. Pol. Chem. Eng. Małgorzata Jaworska / Elżbieta Sikora / Jan OgonowskiReferences1 Kothekar S. C., Waghmare J. T., Momin S. A., Rationalizing and Producing Nanoemulsions for Personal Care. Cosmetics and Toilet-ries, 121(7), 51-56 (2006).2 Sadurni N., Solans C., Azemar N., Garcia-Celma M. J., Studies on the formation of O/W nano-emulsions, by low energy emulsifica-tion methods, suitable for pharmaceutical applications. European Journal of Pharmaceutical Sciences, 26(5), 438-445 (2005). DOI: 10.1016/j.ejps.2005.08.0013 Somasundaran P., Chakraborty S., Deo N., Somasundran T., Nanoencapsulation for Extraction and Release of Fragrance. Cos-metics and Toiletries, 2006, 121(12), 47-54 (2006).4 Usón N., Garcia M. J., Solans C., Formation of water-in-oil (W/O) nano-emulsions in a water/mixed non-ionic surfactant/oil systems prepared by a low-energy emulsification method. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 250(1-3), 415-421 (2004). DOI: 10.1016/j.colsurfa.2004.03.0395 Tadros T., Izquierdo P., Esquena J., Solans C., Formation and stability of nano-emulsions. Advances in Colloid and Interface Sci-ence, 108-109, 303-318 (2004). 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The influence of glicerides oil phase on O/W nanoemulsion formation by pic method

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The influence of glicerides oil phase on O/W nanoemulsion formation by pic method

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Periodica Polytechnica (Budapest University of Technology and Economics)