J. of Supercritical Fluids 83 (2013) 133–145 Contents lists available at ScienceDirect The Journal of Supercritical Fluids jou rn al hom epage: www.elsevier.com/locate/supflu Solvent extraction and purification of rosmarinic acid from supercritical fluid extraction fractionation waste: Economic evaluation and scale-up André Wüst Zibetti a,∗ , Abdelkarim Aydi b , Mayra Arauco Livia a , Ariovaldo Bolzan a , Danielle Barth c a Laboratory of Process Control, Departments of Chemical Engineering and Food Engineering, Universidade Federal de Santa Catarina (UFSC), P.O. Box 476, 88010-970 Florianópolis, SC, Brazil b Laboratoire des Matériaux, Molécules et Applications, IPEST, P.O. Box 51, 2070 la Marsa, Tunisia c Université de Lorraine, Laboratoire Réactions et Génie des Procédés, UMR CNRS 7274, 1 Rue Grandville, BP 20451, 54001 Nancy Cedex, France a r t i c l e i n f o Article history: Received 28 September 2012 Received in revised form 5 September 2013 Accepted 6 September 2013 Keywords: Ultrasound assisted extraction Batch extraction Supercritical fluid extraction and fractionation Rosemary Rosmarinic acid Purification Cost estimation Waste recovery a b s t r a c t Industry is increasingly interested in natural food preservatives, antimicrobial, and antioxidants due to their beneficial effects. The use of plant waste also presented itself to be a great opportunity in recov- ered bioactive compounds remaining in the residue. In this work, bioactive compounds were obtained from Rosmarinus officinalis in two different ways: firstly the supercritical fractionated rosemary extract with different composition was obtained from the plant material, and secondly a potent antioxidant- rosmarinic acid (RA) – was successfully extracted from the plant waste. A purification process scale-up of RA was proposed using GRAS solvent, and an economic evaluation was made for the overall pro- cess. A complete process to obtain bioactive compounds, antimicrobial (supercritical fluid extraction and fractionation extraction) and antioxidant (solvent extraction) was developed. © 2013 Elsevier B.V. All rights reserved. 1. Introduction Bioactive compounds in plants are secondary metabolites that have pharmacological or toxicological effects. There are several compounds that show those types of effects. Rosmarinic acid (RA), carnosol and carnosic acid are important natural antioxidants found in rosemary (Rosmarinus officinalis). There are a number of papers that report the biological activities of this compound, especially RA. Besides potent antioxidant activity, studies have demonstrated that the compound has anti-inflammatory, antial- lergenic, antiviral, and antibacterial functions and shows very low toxicity [1,2]. The antimicrobial and antivirus activities of rose- mary essential oil (EO) have long been acknowledged. The main ∗ Corresponding author at: Departamento de Engenharia Química e Alimentos (EQA), Universidade Federal de Santa Catarina (UFSC), Campus Trindade, 88010- 970, P.O. Box 476, Florianópolis, SC, Brazil. Tel.: +55 48 3721 4073; fax: +55 48 3721 9554. E-mail addresses: azibetti@gmail.com (A. Wüst Zibetti), aydiabdelkarim@gmail.com (A. Aydi), mayarau0@hotmail.com (M. Arauco Livia), abolzan@enq.ufsc.br (A. Bolzan), danielle.barth@univ-lorraine.fr (D. Barth). compounds like -pinene, linalool, 1.8-cineole, camphor, bornyl acetate, borneol and verbenone are suggested due to their antimi- crobial activities [3–8]. Those natural compounds, antimicrobial, and antioxidants are commonly named bioactive compounds [9]. There is a growing interest in using natural antimicrobial and antioxidant in foods [10,11]. The use of “green” processes to obtain these bioactive compounds is attracting attention (despite their higher economic cost) because of its sustainable reasons. Those types of processes also include the use of agricultural solid waste and GRAS (Generally Recognized as Safe) solvent applications [12–15]. There is an increasing number of research related to the extrac- tion of bioactive compounds, including new technologies. Despite these improvements, few works are concerned with reusing solid waste from hydrodistillation or supercritical extraction of herbs using only GRAS solvents. Thus the aims of this present work are: - To evaluate the operational conditions of supercritical fluid extraction and fractionation (SFEF) with cyclonic separators in the obtainment of added value essential oil; 0896-8446/$ – see front matter © 2013 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.supflu.2013.09.005