Microencapsulation of squalene from blue shark liver oil by supercritical CO2 precipitation

Author(s)

Debora Nascimento e Santos

• Document type: Doctoral Thesis
• Press: Pirassununga.
• Institution: Universidade de São Paulo (USP). Faculdade de Zootecnica e Engenharia de Alimentos (FZE/BT)
• Defense date: 2016-06-10

Examining board members

Alessandra Lopes de Oliveira; Reinaldo Camino Bazito; Rosemary Aparecida de Carvalho; Maria Angela de Almeida Meireles; Samantha Cristina de Pinho

• Advisor: Alessandra Lopes de Oliveira

Abstract

Blue shark liver oil has a high nutritional value and is rich in numerous active substances, such as squalene, vitamin A, polyunsaturated fatty acids. The purpose of this study was to obtain blue shark liver oil (Prionace glauca) under mild temperature conditions using supercritical fluid extraction (SFE) and to study the microencapsulation process of the oil using the particle formation system from gas saturated solution/suspension (PGSS). To study the supercritical extraction parameters of blue shark liver oil (BSLO), cobia liver (Rachycentron canadum) was used as a model and supercritical extractions were performed at different conditions of temperature (T, 50, 60 and 70 °C) and CO2 flow rate (5, 8 and 11 g CO2/min), under the same pressure (P) of 250 bar. Considering the higher yield conditions, it was set for the blue shark liver one complete block design with 5 levels of P (100, 150, 200, 250 and 300 bar) and 2 T levels (50 and 60 °C). With the different BSLO, cobia liver oil (CLO) and purchased shark liver oil (PSLO), physicochemical measurements (density, viscosity, refractive index, acid number, peroxide value and saponification number) were performed and the active of interest in this study (squalene, vitamin A and essential fatty acids) were quantified. The BSLO with the highest squalene content was used for microparticle formation step by the PGSS technique in which particles were generated using modified starches as impregnation agents (Hi Cap® 100 and Purity Gum Ultra®) and characterized. CLO had different yields, ranging from 40 to 58%, when different operating conditions were applied and these results contributed to the definition of extraction conditions of BSLO. The physicochemical characteristics were consistent with oils without refining, highlighting the high acid content (13.6 to 17% oleic acid), which was considered characteristic of CLO. The CLO has high biological value fatty acids. The levels of monounsaturated fatty acids were 41.2 to 49 g/ 100 of CLO and polyunsaturated fatty acids ranged from 21.8 to 25.3 g/ 100 g of CLO. Squalene in oils ranged 354 - 462 mg/ 100g of CLO, reinforcing the potential of this matrix for several applications. BSLO yields of extractions ranged 0-60%, considered for the highest values superior to conventional methods. BSLO showed physicochemical parameters such as density from 0.920 to 0.922 g.mL-1, viscosity from 52 to 56 Pa.s, refractive index of 1.4760 to 1.4785, acid number from 1.1 to 2.2% oleic acid, peroxide value from 10 to 24 meq of active O2/ kg of BSLO and saponification number of 171-534 mg KOH/ kg of BSLO comparable to refined fish oils. The squalene and vitamin quantification assays indicated values of 161.30 to 542.55 mg of squalene/ 100g of BSLO and 579-3,682 retinol equivalent/ g of BSLO. The generated microparticles showed considerable oil retention index on the surface, 74-82% and, in addition, parameters such as low hygroscopicity and high solubility of modified starches makes these particles widely applicable in the food area. The behavior study of modified starches Hi Cap® 100 and Purity Gum Ultra® in contact with supercritical CO2 has not indicated volumetric expansion in the samples under the conditions evaluated. Although the oil extracted with supercritical CO2 had refined oils characteristics, analyzes the stability of the microparticles showed the necessity of refining for greater shelf life of the product. Squalene found decreased along the stability study period (0 to 60 days), however, it was found in every day and analyzed in all treatments. The squalene content, the compound found in every day and for all treatments analyzed, decreased along the stability study period (0 to 60 days). (AU)

• FAPESP's process: 12/00467-3 - MICROENCAPSULATION OF SQUALENE FROM DOGFISH LIVER OIL THROUGH PRECIPITATION WITH SUPERCRITICAL CO2 USING THE RESS TECHNIQUE
• Grantee: Débora Nascimento e Santos
• Support Opportunities: Scholarships in Brazil - Doctorate