22 Microwave Assisted Extraction
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1 22 Microwave Assisted Extraction The most widely described application of microwave treatment in organic materials processing has been microwave assisted extraction. In this method, plant materials such as wood, seeds and leaves are suspended in solvents and the mixture is exposed to microwaves instead of conventional heating. Enhanced rates of extraction for plant based oils have been observed for a range of plant materials. All microwave-assisted extraction techniques can be considered an alternative to conventional techniques because they reduce: extraction times; costs; energy; solvent consumption; and CO 2 emissions (Chemat and Cravotto 2013). In addition, some techniques have been successfully applied at an industrial scale in the cosmetic, perfume, and nutraceutical industries (Chemat and Cravotto 2013). This chapter outlines some examples of microwave assisted extraction Solvent based Extraction of Essential Oils Microwaves assisted extraction maintains mild conditions and usually provides superior extraction; however, apart from laboratory trials, essential oil extraction using microwave energy has had limited commercial development. There are two problems to overcome in the extraction from solid plant materials: that of releasing the essential oil from solid matrix and letting it diffuse out successfully in a manner that can be scaled-up to industrial volumes (Ramanadhan 2005). Chen and Spiro (1994) examined the extraction of the essential oils of peppermint and rosemary from hexane and ethanol mixtures using pulsed microwave energy and found that yields were more than one third greater than from conventional steam distillation techniques. They found that 10 s pulses and 5 minute cooling intervals using 90 % ethanol provided the greatest overall oil yield of a-pinene, with 30 s pulses and 5 minute cooling intervals in hexane providing the second highest yield. The dielectric properties of ethanol are j 7.1 while the dielectric properties of hexane are j (Chen and Spiro 1994). The dielectric properties of rosemary and peppermint leaves are j 4.3 and j 1.3 respectively (Chen and Spiro 1994). Therefore it is expected that ethanol will heat faster than the leaf material wile hexane will heat slower than the leaf material when exposed to microwave fields. Based on temperature data acquired using an IR pyrometer, Chen and Spiro (1994) found that the temperature of peppermint and rosemary leaves was lower than that of the solution by 4 to 12 C when hexane was used for the solvent. Saoud et al. (2006) studied microwave enhanced extraction of essential oils from tea leaves and achieved higher yields (26.8 mg g -1 ) than steam distillation (24 mg g -1 ). Chemat et al. (2005) studied the extraction of oils from limonene and caraway seeds and found that microwave assisted extraction led to more rapid extraction as well as increased yields. Microwave assisted extraction yielded 32 compounds
2 Solvent Free Extraction of Essential Oils 281 in the caraway seed oil, while steam distillation yielded only 18 compounds. Scanning electron microscopy of the microwave treated and untreated seeds revealed significantly increased rupture of the cell walls in the treated seeds. Microwave assisted extraction also led to a more chemically complex extract, which was thought to be a better representation of the true composition of the available oils in caraway seed. Cardoso-Ugarte, et al. (2013) demonstrated that the amount of solvent and heating time significantly affected the yield of essential oils from basil (Ocimum basilicum) and epazote (Chenopodium ambrosioides). They found that basil essential oil yield was not significantly different from steam distillation yields; however epazote essential oil yield was significantly higher than the oil yield obtained by steam distillation. In both cases, microwave assisted extraction required much less time and yielded a richer chemical mixture than steam distillation methods Solvent Free Extraction of Essential Oils Solvent-free microwave extraction is a combination of microwave heating and dry distillation, performed at atmospheric pressure without added any solvent or water. Isolation and concentration of volatile compounds are performed by a single stage. Lucchesi, et al. (2004) compared this technique with conventional steam distillation, for the extraction of essential oil from three aromatic herbs: basil (Ocimum basilicum L.), garden mint (Mentha crispa L.), and thyme (Thymus vulgaris L.). The solvent free method yields an essential oil with higher amounts of more valuable oxygenated compounds, and allows substantial savings of costs, in terms of time, energy and plant material. The energy required to perform the two extraction methods are respectively 4.5 kwh for steam distillation and 0.25 kwh for solvent free microwave extraction. Steam distillation required an extraction time of 270 min for heating 6 kg of water and 500 g of plant material to the extraction temperature, followed by evaporation of water and the essential oil. The solvent free microwave extraction required only 30 min of heating the plant matter and evaporation of the in situ water and essential oil of the plant material. Singh, et al. (2014) compared extraction of essential oil from lemongrass using microwave-assisted hydrodistilation (using water as a solvent) and solvent free microwave extraction. Their results showed that oil yield increases with increasing microwave power, irradiation time and decreasing particle size. The maximum oil yield in microwave-assisted hydrodistilation was 1.72% after 90 minutes of heating and 1.61% in solvent free microwave extraction after 20 minutes of irradiation time. Longer irradiation time resulted in inferior quality of essential oil. Extraction using the solvent free technique was much faster than microwave-assisted hydrodistilation.
3 282 Microwave Assisted Extraction 22.3 Microwave Pre-treatment Followed by Conventional Extraction Techniques Although less well described in the literature, an alternative approach for utilising microwave heating of plant based materials has been to treat the materials prior to extraction. In a study by Miletic et al. (2009), greenery and fruits of conifers were treated in a conventional microwave prior to hydro distillation to extract essential oils. Both the kinetics of hydro distillation and oil yield were significantly increased for plant materials treated with microwaves Application to Sugar Juice Extraction In a recent scoping study (Roberts 2010), sugar cane segments (without nodes) were exposed to varying levels of microwave treatment, in a conventional microwave oven, prior to sucrose diffusion in water at 65 o C for 60 minutes, which demonstrated that microwave treatment of cane prior to diffusion led to significant decreases in colour and significant increases in purity and pol. Qualitative observations indicated faster rates of extraction in the microwave treated cane; however decreases in juice quality was observed for long microwave treatment times, indicated that an optimum treatment time existed. In another simple scoping experiment, sugar cane billets were randomly allocated to one of four microwave pre-treatments (0, 90, 120, or 150 seconds) in a low powered domestic microwave oven before being crushed in a small press made from a manual screw type car jack. There was a significant increase in cane juice yield as a result of microwave treatment (Table 22.1). The 120 seconds treatment yielded the greatest amount of sugar juice; however there was a significant decline in yield as microwave treatment increased to 150 seconds. This is probably due to excessive drying of the cane billets. The samples that were treated for 120 seconds yielded approximately 3.2 times more cane juice than the untreated control samples. This additional yield from the microwave pre-treatment of sugar cane samples is probably due to several factors: 1. a significant softening of the woody polymers (cellulose, hemi-cellulous and lignin) as the internal temperature of the cane billets rose above their respective glass transition temperatures (Manríquez and Moraes 2010). Brodie et al. (2011) found that microwave pre-treatment of sugar cane reduced the compressive strength of the cane to about 18 % of its original strength (the control samples); 2. rupture of the internal cellular structures in the cane due to localized steam explosions induced by microwave heating (Vinden and Torgovnikov 2000); and 3. a reduction in viscosity of the sugar juice.
4 Microwave Accelerated Steam Distillation 283 Table 22.1: Mean sugar juice yield as a percentage of initial cane billet mass. Treatment Yield (%) Control 8.4a 90 s 26.5b 120 s 26.8b 150 s 18.1c LSD (P = 0.05) 8.2 Note: Means with different superscripts are significantly different from one another Microwave Accelerated Steam Distillation Chemat et al. (2006) developed a new process design and operation for microwave accelerated steam distillation of essential oils from lavender flowers (Lavandula angustifolia). In this system, the lavender flowers sit above the steam source generated by microwave heating. Only steam passes through the flowers without the boiling water mixing with vegetable raw material, as is the case in conventional hydro-distillation. Microwave accelerated steam distillation was compared with a conventional technique, steam distillation, for the extraction of essential oil from lavender flowers. Extraction of essential oils from lavender with microwave accelerated steam distillation was better than conventional steam distillation in terms of energy saving, rapidity (10 min versus 90 min), product yield, cleanliness and product quality. Chemat et al. (2006) treated 50 g samples of lavender flowers, which required 5.4 MJ of energy for conventional steam distillation (or 180,000 MJ tonne -1 ). Microwave accelerated steam distillation required 0.47 MJ of energy to achieve full distillation of the 50 g samples (or 9,400 MJ tonne -1 ). The composition of the final oil from each treatment regime was very similar; therefore the faster extraction using microwave energy did not affect the product quality. In a small trail, a 10 kw, 922 MHz, microwave system was used to treat 10 kg samples of tea tree (Melaleuca alternifolia) leaf material to distil tea tree oil. These experiments were conducted in a rotating microwave chamber, which tumbled the leaf material during microwave processing. Water was added to the leaf material at a rate of 20 % by mass to facilitate good steam generation to transport the oil vapour to the condenser. Estimated energy requirements for this process were 3,850 MJ tonne -1.
5 284 Microwave Assisted Extraction References Brodie, G., Jacob, M. V., Sheehan, M., Yin, L., Cushion, M. and Harris, G Microwave modification of sugar cane to enhance juice extraction during milling. Journal of Microwave Power and Electromagnetic Energy. 45(4): Cardoso-Ugarte, G. A., Juarez-Becerra, G. P., Sosa-Morales, M. E. and Lopez-Malo, A Microwave-assisted extraction of essential oils from herbs. Journal of Microwave Power & Electromagnetic Energy. 47(1): Chemat, F. and Cravotto, G Microwave-assisted extraction for bioactive compounds. Theory and practice. Food Engineering Series Chemat, F., Lucchesi, M. E., Smadja, J., Favretto, L., Colnaghi, G. and Visinoni, F Microwave accelerated steam distillation of essential oil from lavender: A rapid, clean and environmentally friendly approach. Analytica Chimica Acta. 555(1): Chemat, S., Aït-Amar, H., Lagha, A. and Esveld, D. C Microwave-assisted extraction kinetics of terpenes from caraway seeds. Chemical Engineering and Processing. 44(12): Chen, S. S. and Spiro, M Study of microwave extraction of essential oil constituents from plant materials. Journal of Microwave Power and Electromagnetic Energy. 29(4): Lucchesi, M. E., Chemat, F. and Smadja, J Solvent-free microwave extraction of essential oil from aromatic herbs: comparison with conventional hydro-distillation. Journal of Chromatography A. 1043(2): Manríquez, M. J. and Moraes, P. D Influence of the temperature on the compression strength parallel to grain of paricá. Construction and Building Materials. 24(1): Miletic, P., Grujic, R. and Marjanovic-Balaban, Z The application of microwaves in essential oil hydro-distillation processes. Chemical Industry and Chemical Engineering Quarterly. 15(1): Ramanadhan, B Microwave Extraction of Essential Oils (from Black Pepper and Coriander) at 2.46 GHz. Unpublished thesis. Canada: University of Saskatoon, Saskatchewan, Department of Agricultural and Bioresource Engineering Roberts, I Analysis of the effects of micrwave treatment on sugarcane diffusion products. Unpublished Undergraduate thesis. Townsville: James Cook University, Engineering Department Saoud, A. A., Yunus, R. M. and Aziz, R. A Yield study for extracted tea leaves essential oil using microwave-assisted process. American Journal of Chemical Engineering. 6(1): Singh, N., Shrivastava, P. and Shah, M Microwave-assisted extraction of lemongrass essential oil: Study of the influence of extraction method and process parameters on extraction process. Journal of Chemical & Pharmaceutical Research. 6(11): Vinden, P. and Torgovnikov, G The physical manipulation of wood properties using microwave. Proc. International Conference of IUFRO Tasmania, Australia.
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