The production of essential oils from rosemary (Rosmarinus officinalis)result the formation of lignocellulosic waste, not easily biodegradable andinvolve environmental problems. In this work we developed process toproduce monomeric sugars with high added value from this waste, after thetreatment respectively with the vapour (10min, 205°C under 1 bar) and acidhydrolysis ( sulphuric acid 0.5%).The acid hydrolysis thereafter, improved by pretreatments (explosion bythe steam of water), permits to damage all polymers recalcitrant to theacidic hydrolysis

CHAOUCH, M.

EL YEMNI, M.

ELOUTASSI, N.

LAHKIMI, A.

LOUASTE, B.

Revues Scientifiques Marocaines

J. Appl. Sci. Envir. Stud. 1(1) (2018) 16-20  El Yemni et al., J. Appl. Sci. Envir. Stud. 2018, 1 (1), pp. 16-20 16 !!  Journal of Applied Science and Environmental Studies JASES http://revues.imist.ma/index.php?journal=jases !!   Valorization of the wast descended from the hydrodistillation of Rosmarinus officinalis  Majda EL YEMNI 1, Noureddine ELOUTASSI 1, Amal LAHKIMI 1, Bouchra LOUASTE 2, Mahdi CHAOUCH 1 1Laboratory of Materials and Environment Engineering, Faculty of Sciences Dhar El Mehraz, USMBA, Fez 2Biotechnology Laboratory, Faculty of Sciences Dhar El Mehraz, USMBA.Fes   Received 15 June 2018 ; Revised 25 Aug 2018, Accepted 28 Aug 2018  Keywords  Rosmarinus officinalis Steam treatment Acid and hydrolysis.  Abstract The production of essential oils from rosemary (Rosmarinus officinalis) result the formation of lignocellulosic waste, not easily biodegradable and involve environmental problems.  In this work we developed process to produce monomeric sugars with high added value from this waste, after the treatment respectively with the vapour (10min, 205°C under 1 bar) and acid hydrolysis ( sulphuric acid 0.5%).  The acid hydrolysis thereafter, improved by pretreatments (explosion by the steam of water), permits to damage all polymers recalcitrant to the acidic hydrolysis. !1.! Introduction Lignocellulosics contain sugars polymerised to cellulose and hemicellulose which can be liberated by hydrolysing the material, and then fermented to ethanol by microorganisms, e.g. Saccharomyces cerevisiae, candida tropicalis, Pichia Stipitis [1]. The biological ethanol can be regarded as a more environmentally friendly fuel than gasoline because it adds only little net carbon dioxide to the atmosphere. This is the main reason why large research efforts are done to find a cheap way of producing ethanol from renewable raw materials [2; 3].  The work presented in this paper was performed to elaborate treatment process on Rosmarinus officinalis essential oils hydrodistilation waste  J. Appl. Sci. Envir. Stud. 1(1) (2018) 16-20  El Yemni et al., J. Appl. Sci. Envir. Stud. 2018, 1 (1), pp. 16-20 17 !  2.! Materials and methods  2.1.Preparation of the lignocellulosic hydrolysate  Hydrodistilation by product biomass (1Kg) of Rosmarinus officinalis was washed with water and filtered in filter press unit at a pressure of 10 bar. The filtrate was collected and subjected to steam pretreatment at 205 C° for 10 minutes. The steam treated residual is diluted in sulphuric acid, and then it is maintained to the heating during 50 min. Detoxification is achieved by increasing pH to 9 with Ca(OH)2 (room temperature, magnetic stirrer for 2 h) after which the solution was filtered through a 0.45 µm Millipore filter and the pH was adjusted pH 7 with concentrated H2S04.  2.2.Analysis The phenol-sulfuric acid method was used for measuring a broad spectrum for carbohydrates, [4]. Total phenol was analyzed according to a modification of the Folin-Ciocalteau method [5].  3.!Results and discussion The experimental programme was divided chronologically into two different phases. During the first phase, the pre-treatment process of substrate was elaborated by means of primary (steam and acid hydrolysis) and secondary treatments (detoxification) to permit further ethanol bioconversion. 3.1.Treatment procedure Various methods for the hydrolysis of lignocellulosic materials for ethanol   production have recently been described [1]. In this work steam hydrolysis and dilute-acid hydrolysis will be measured. a.! high-temperature steam treatment Prior to acid hydrolysis, the cellulose structure must be made available to the hydrolysing acids by subjecting the material to some form of pre-treatment. Wood can be pre-treated using high-temperature steam which solubilises the hemicelluloses [6]. From figure 1, we noticed that great fraction of total phenolic compounds are liberated from hydro-distilled biomass. The release of sugars is not a sufficient amount when compared to phenolic compounds.   a.! Diluted acid hydrolysis  Optimal concentration of sulphuric acid (0.5%) has been added to plant biomass waste (100g). As means of measurement the liberation of the reducing sugars and phenolic compounds has been followed.   J. Appl. Sci. Envir. Stud. 1(1) (2018) 16-20  El Yemni et al., J. Appl. Sci. Envir. Stud. 2018, 1 (1), pp. 16-20 18 ! Fig 2: Liberation of total sugars and total phenolic compounds during  the time of the steam pre-treatment .  Table 1: Liberation of total sugar and phenols according to the sulphuric acid concentration during 50min acidic hydrolysis. Sulfuric acid (%) total sugar gl-1 Phenolic compounds gl-1 0.1 10.85 14.25 0.5 17 14.25 1 17 14.25 2 17 14.25 5 17 14.25 10 17 14.25 20 17 14.25  From table 1 we noticed that 0.1% of acid release the totality of phenolic compounds, whereas a concentration of 0.5% is sufficient to release the majority of the monomeric sugars contained in polymeric carbohydrate in the plant waste.   Dilute-acid hydrolysis is fast and easy to perform and the ethanol yields obtained is only 30-50% of the theoretical values (unpublished results) so technical detoxification was called out to increase the yield of fermentation.   0123456789100 2 4 6 8 10Concentration!(g/l)time!(min)Total!sugars Phenolic!compoundsJ. Appl. Sci. Envir. Stud. 1(1) (2018) 16-20  El Yemni et al., J. Appl. Sci. Envir. Stud. 2018, 1 (1), pp. 16-20 19 !b.! Detoxification Detoxification methods can be developed for efficient removal of inhibitors prior to fermentation of strongly inhibiting hydrolysates in rosemary biomass after hydrodistilation.  Ca(OH)2 has been tested for its well-known precipitation characteristics with regard to acid and phenolic compounds substances, including several inhibitors of hemicellulose fermentation.  The phenolic compounds elimination was very important (60%) and fermentation was improved by 40% (unpublished results). From these results we noticed that the detoxification reduces a great part of inhibitors of the alcoholic fermentation (tab. 2). Table 2:  Evolution of Sugar composition during all the steps of Rosmarinus officinalis biomass testament. Sugars  Distillation Vapour treatment  Hydrolyse acid Detoxification  Glucose (g/l) 6.05 6.55 9.6 9.5 Xylose (g/l) 2.02 2.25 7.33 7.2 Manose (g/l) 0.015 0.02 2.37 2.37 Galactose (g/l) 0.225 0.25 1.2 1.2 Cellulose  Hemicellulose (g/l) 8.8 9.2 0 0 Total phenolic compounds (g/l) 2.5 5.1 14.25 5.8  Sugars production yields were improved gradually from distillation, steam pretreatment and acidic hydrolysis procedure. The effects are revealed in Table 2. The best results have been obtained at acidic hydrolysis. Direct acidic hydrlysis did not give the same results. This procedure resulted in an increase the yield of sugars up to 9.6 of glucose, 7.33g/l of xylose, 2.37 g/l of mannose, and 1.2g/l of galactose. These values are more important than those observed in steam treatment.  The firsts steps in the process are the distillation of essential oil, prehydrolysis (steam pre-treatment) and acidic hydrolysis (fig1 and table 1). In these steps the lignocellulose is delignified and a depolymerisation takes place. During the acid hydrolysis not only free sugars are formed (table 1), but also inhibitors, like acidic and phenolic compounds.  References 1.! Olsson, L and Bärbel Hahn Hägerdal (1996). Fermentation of lignocellulosic hydrolysates for ethanl production. Enzyme and Microbial Technology., 18, 312-331. J. Appl. Sci. Envir. Stud. 1(1) (2018) 16-20  El Yemni et al., J. Appl. Sci. Envir. Stud. 2018, 1 (1), pp. 16-20 20 !2.! Whitten, G. Z., J. P. Cohen, A. M. Kuklin. 1997. Regression Modeling of Oxyfuel Effects on Ambient CO Concentrations. Prepared for Renewable Fuels Association, and Oxygenated Fuels Association. http://www.ethanolrfa.org/967810.html. 3.! Nunes, A. P., J. Pourquie. 1996.  Steam Explosion Pretreatment And Enzymatic Hydrolysis of Eucalyptus Wood. Bioresource Technology  57: 107-110. 4.! 12- Dubois, M.,A.K.Gilles, J.K.Hamilton, P.A.Rebers, and F.Smith. Colorimetric method for determination of sugars and related substances. Anal. Chem. 1956, 28, 350-356 5.! 11- Box, D, J., Investigation of the folin ciocalten phenol reagent for the determination of polyphenolic substances in natural waters. Water Ress 1983, 17, p.511 6.! Kim Kyoung Heon, Melvin P.Tucker, Fred A.Keller, Andy Aden, Quang A.Nguyen. 2001. Continous contercourrent extraction of hemicellulose from pretreated wood residues. Applied Biochemistry and biotechnology, 91, 93, 253-267 !!!!!!!!!!(2018) © JASES, USMBA Fez, Morocco 

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Valorization of the wast descended from the hydrodistillation of Rosmarinus officinalis

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Valorization of the wast descended from the hydrodistillation of Rosmarinus officinalis

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