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Ultrasonics Sonochemistry 8 (2001) 303±313

An overview of the ultrasonically assisted extraction of
bioactive principles from herbs
Mircea Vinatoru *
``Costin D. Nenitzescu'' Institute of Organic Chemistry, Romanian Academy, P.O. Box 15-254, 77141 Bucharest, Romania

This paper presents a review of the ultrasonically assisted extraction of bioactive principles from herbs. Much of the work was
carried out under European community grants under the COPERNICUS programme and in a COST D10 network. Some aspects of
classical and non-conventional extraction procedures are also presented and brie¯y discussed. Ó 2001 Elsevier Science B.V. All
rights reserved.

Keywords: Ultrasonic extraction; Tinctures; Ultrasonic swelling index; Ultrasonic extractive value

1. Introduction A herbal extract could be de®ned as the compounds
and/or compound mixtures obtained from fresh or dried
Vegetal materials are invaluable resources, useful in plants, or parts of plants: leaves, ¯owers, seeds, roots
daily life as food, food additives, ¯avors, fragrances, and barks, by di€erent extraction procedures. Charac-
pharmaceuticals, colors or directly in medicine. This use teristically, the active constituents are obtained together
of plants has a long history all over the world and, over with other materials present in the vegetal mass. The
the centuries, humanity has developed better methods extraction of bioactive components from vegetal ma-
for the preparation of such materials. Nowadays, there terials is part of phytopharmaceutical and food technol-
is a renaissance of interest in natural remedies, in part ogy.
due to some disillusionment with modern medicine and It is obvious that herbal preparations are of great
drugs that either do not perform entirely to expectation medicinal interest, and for this reason herbal prepara-
or are accompanied by unwanted side e€ects. Natural tions, which include herbal extracts, were introduced in
remedies have the advantage that they have passed the the pharmacopoeias of numerous countries, Table 1 [1].
proof of time. On the other hand some synthetic drugs Medicinal and aromatic plants provide an inex-
even though they have been used for over 100 years, haustible resource of raw materials for the pharmaceu-
may still need more time to be proven to be absolutely tical, cosmetics and food industries and more recently in
harmless. agriculture for pest control [2]. People have learned to
Perhaps anyone not familiar with the problems re- increase the power or usefulness of herbs by preparing
lated to medicinal herbs might consider this subject medicinal compounds from them, by preserving them so
unimportant, or of only minor importance. Others that they are always available, and by ®nding new ways
may feel that, in a period in which synthetic and highly to release their active constituents. Among modern
ecient drugs are available for treatment of various methods used to release the bioactive constituents from
diseases, medicinal herbs have become archaic and rep- herbs is ultrasonically enhanced solvent extraction. The
resent only a centuries-old tradition. Others however use of ultrasound to enhance the extraction yield is a
consider them a form of natural remedy to oppose technique that started in the 1950s with laboratory scale
modern drug consumerism. experiments [3].
To make an extract, ®rst of all it is important to
identify the desired herb and the part of it which con-
Tel.: +40-1-637-5948; fax: +40-1-312-1601. tains useful constituents, but this is not so simple.
E-mail address: (M. Vinatoru). Around 350 years ago, one of the most famous English
1350-4177/01/$ - see front matter Ó 2001 Elsevier Science B.V. All rights reserved.
PII: S 1 3 5 0 - 4 1 7 7 ( 0 1 ) 0 0 0 7 1 - 2

the discovery of new applications of various herbal constituents. In the Greek and methods are available: Roman empires there was an expanding process for the therapeutic use of herbs.g. However for chemists an ill person ®rst use psychotherapy. The expression ``folk medicine''. in the second century. Paracelsus. The ®rst use was for nutrition. even though it may 2. city [7]. water''. Egyptian papyruses describe thousands of recipes showing that coriander and castor oils were used for 3. A short history of plants and plant extract uses have pejorative overtones. of these compounds were introduced into industry e. the British pharmacopoeia 80 hospital ÔColteaÕ included a pharmacy selling medicinal Scandinavian pharmacopoeia 80 herbs. herbal products were intro- International pharmacopoeia 45 duced in the Romanian pharmacopoeia and in 1904 the ®rst institute of medicinal herbs was established in Cluj herbalist Culpeper. discovered initially as salicylic acid in willow Actually. in the 16th century made an (b) maceration with solvent. used in Europe. the me.304 M. To obtain extracts from vegetal materials several with details that are useful today. (b) water steam distillation. actually means centuries of empirical experiments and over a hundred years of sci- The history of vegetal materials use is as old as hu. described in a wonderful book sev. time as well as the preserving methods are of crucial The interest in medicinal and aromatic herbs has importance and therefore a precise technique must be revived with the identi®cation of new compounds and setup for this purpose [5]. known since 1380 was the ®rst alcoholic extract 2. when research work for developing new bark and leaves. the chemical content of herbs failed use. . In French pharmacopoeia 190 the 19th century French researchers extended investi- Switzerland pharmacopoeia 180 gations into the ®eld of herbal products. seeds. In the 19th century. His rules are still applicable today and readers tories for the synthesis of medicinal compounds. Nowadays after phytotherapy. Indeed. ``Hungarian (c) water and steam distillation. thyme.C. in (a) direct essential oil distillation. Some will ®nd them useful in the gathering of leaves. Galenus described. enti®c research. Otopeni). cosmetics and preservatives. introducing aromatic and medicinal Country Number of herbal herbs to a ``hot bath'' (this is still in use today in Ro- drugs monographs mania at the Ana Aslan Geriatric Institute. around 30 papers and recipes. these being the ultrasonically assisted extraction of troduced into agriculture for their essential oils or their bioactive principles. He- brew and Chinese manuscripts describe over 2000 herbs.. sent day. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 Table 1 important contribution to the study of aromatic and Entries on herbal drugs in pharmacopoeias medicinal herbs. such as lavender. For example the herb ÔMother- Hungarian pharmacopoeia 110 wortÕ (Leonurus cardiaca) was mentioned by Herodotus Romanian pharmacopoeia 105 Italian pharmacopoeia 105 (5th century B. For industrial modern medicine introduces chemotherapy (synthetic processing medicinal and aromatic herbs. aspirin. hyssop. Soon. the harvesting drugs) as another step before surgery. Extraction procedures medicinal application. eral rules for gathering plant parts for herbal prepara. setting up USSR pharmacopoeia 140 Polish pharmacopoeia 125 procedures to obtain the desired extracts driven by the British codex 125 growing demand for perfumes. initially from written forms throughout many generations to the pre- natural and later from cultivated ¯ora. one of herbs. Several bring it to light by using modern methodologies. extensively (a) solvent extraction (percolation). then if there are no not familiar with botany this could prove to be a very results use phytotherapy and. only if these two therapies dicult task. Distillation: content. which has become one of the most used extraction techniques starts up. were in. gathered and transmitted by oral and manity. barks and other parts. strongly depends on the gathering time. According to Hippocrates for healing is to gather the required herbs. surgery. It is our duty to use this information and to dicinal properties of herbs were discovered. roots. Solvent extraction: from rosemary. and was. In 1700 in Bucharest. Belgian pharmacopoeia 120 In Romania the use of medicinal herbs has been Holland pharmacopoeia 120 known since antiquity.) in his writings about people living German pharmacopoeia 85 north of the Danube river [6]. It is well known that plants provide perfect labora- tions [4]. medicinal compounds. ¯owers. for ®ve centuries. dicinal purposes which are still up to date. etc. the ®rst thing to be done industrial drugs. herbal extracts for me. mainly for their essential oil 1.

Non-conventional extraction techniques: (a) supercritical ¯uid extraction.34 CE: classical extraction (Soxhlet).50 7 days M ‡ 30 min US 25.3. the yield of extracted com- centers.1. 3. From the times. ultrasound can be successfully employed to 3. Here the but the mechanism not yet understood. This is possible because in almost all cases solvent extraction uses cold solvent (percolation can be done with cold as 3. the liquid is transferred that maceration prevents more limonene being extracted though a throttle 5 into the separation unit 2. This yields a crude essential oil obtained by classical or maceration methods. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 305 (c) boiling with water (infusion).40 60 min 51.40 0.00 240 min 40.84 0.77 65. the carbon dioxide gas after passage through a traction …US† ‡ 240 min re¯ux (R)] the concentration of heat exchanger and ®lter (4 and 7) is compressed in the limonene decreases even when ultrasound is used.28 65. One of the most liquid carbon dioxide is heated to reach the gaseous Table 2 Comparison between di€erent extraction methods of 100 g of dill seeds. obtained via classical or ultrasound extraction. A distillation unit provided with borneol. Table 3 shows that when using so- troduction of water steam. important observations in this case is that ultrasonically (d) extraction with cold fat (en¯eurage). Solvent extraction procedures. These studies can o€er similar or better extracts [8.79 47. However. excluding fat extrac- (b) vortical (turbo) extraction. can be achieved simply by the introduction of an ul- (d) ultrasonically assisted extraction.34 M ‡ US ‡ R 3. 3. assisted extraction leads to non-detectable amounts of (e) extraction with hot fat. It seems After completing the extraction. An example showing how extraction techniques that can o€er very good yields. US: ultrasonic extraction. the authors follow the individual compo- traction techniques such as extraction with light solvents nents of sage extraction [10]. are more amenable to ultrasonic treatment.40 30 min 49. M: maceration. R: re¯ux. bottle 8. trasonic transducer into the extraction unit. % CE 3.69 0. This is the main proce- In another example of ultrasonically assisted solvent dure for obtaining essential oils. but no collapsing bubbles.2. clearly show that a probe system is a better sonication During distillation it is obvious that the use ultra- technique for the extraction of cineole.92 0.15 ± US 3. Distillation well as with hot solvent).22 45. which is the usual method for the natural oil industry.9]. [7 days maceration …M† ‡ 30 min ultrasonic ex. and the temperature of the extraction mixture is Extraction with supercritical ¯uid is one of the newer kept below its boiling point. if any. Cold compression. M.84 ± M ‡ US 3. A typical scheme for a super- It is interesting to note that at longer extraction critical extraction unit is given in Scheme 1.10 M ‡ US ‡ R 3.29 0.08 66. and cooled again until reaching the liquid quite strange since the amount of oil is greater than that state when it is introduced into the extraction unit 1.55 7 days M ‡ 60 min US ‡ 240 min R 20. improvement in yield. tion. Even when using a cleaning bath as the ultra- an ultrasonic source will produce more rapidly boiling sonic device for extraction. but some other ex- extraction. ¯uid is carbon dioxide. ultrasound can help solvent extraction of essential oils For this procedure the most often used supercritical from di€erent vegetal materials is given in Table 2 [8]. Therefore this kind pounds rose to near completion. .05 M ‡ US 3. This is compressor 3.72 65.55 7 days M ‡ 30 min US ‡ 240 min R 20.09 US 3. of unit will be useful only to enhance boiling with little.63 48. Non-conventional extraction techniques enhance extraction when low boiling point solvents are used. heavy components. thujone and sonic energy is futile. Table 4. Solvent extraction 4. that should be further distilled.50 7 days M ‡ 60 min US 20. This (c) extraction by electrical energy. using hexane Method used Oil amount (g) Extraction time Components Limonene % Carvone % Heavy comp. Table 3 contains results showing the e€ect of ultra- Distillation means that vegetal materials are mixed sound on dry residue yield for several medicinal and (or not) with water followed by heating or by the in- aromatic plants [9]. The resulting vapors are nication the content of dry residue (which measures cooled and collected in a separator and the essential oil total extract) is either similar to or greater that that separates from water.

This new Cannabinol 310 90 Tetrahydrocan.3 Silent control experimentb 14.91 1.58 0. b Probe system.33 1.6 Cleaning bath ‡ stirrera 22.36 ± 0.5 118.7 141.91 1.50 4.9 6. removed.25 Classical 7±14 days 1.25 1.10 0. enhancing thereby the extraction yield.78 1.98 1.94 ± 30 0. b Best silent results.80 ± ± ± ± ± 18 h maturation 0. Table 6 [13]. Scheme 1.06 2.306 M.6 6.73 1.94 1.43 0. The vortical (turbo) extraction procedure uses a high formed.75 2.74 90 0. This technique is suitable for fragrance extrac.92 0. using tetra¯uoroethane leaves Menthone 156 70 as the working solvent.56 0. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 Table 3 Dry residue (g/100 g extract) obtained by direct sonication Sonication time (min) Minta Camomilea Sagea Arnicaa Gentiana Marigolda Marigoldb 15 0.71 1.5 a For these procedures data were collected at 3 h.80 0.02 1.30 0. tion. 315 90 extraction technique combines the advantages of su- nabinol percritical ¯uid extraction with those of normal solvent extraction. In Scheme 2 a simpli®ed dia.25 a Cleaning bath. selective extractions can be per.79 1.97 120 0.8 Cleaning batha 16.67 0.07 1.3 167. Triglycerides >600 90 A technique resembling supercritical ¯uid extraction Peppermint Menthol 158 70 is that developed by Wilde [12]. state.15 60 0.15 1.0 176.06 1. and from the bottom of the vessel the Table 5 extract is drawn o€ through the valve 6a. Cannabis Cannabidiol 314 85 gram of a possible extraction unit is given.25 180 ± 1. speed stirrer that induces hydrodynamic cavitation. Table 4 Comparison of di€erent ultrasonic extraction procedures for sage Extraction procedure Component extracted (mg/kg) Cineole Thujone Borneol Probe (2 h) 24.68 2.20 3.66 1.14 1.75 2. Using di€erent combinations of ¯uoroethane with organic solvents.75 4.24 1. Supercritical extraction (selected examples) An example of the use of supercritical extraction Herb.02 1.2 5. It is . Schematic diagram of supercritical ¯uid extraction unit. From this example weight at (bar) one can see that using di€erent pressures of supercritical Caraway seeds Limonene 136 70 Carvone 160 70 ¯uid a selective extraction can be performed.20 2.67 2.1 3.42 1.82 1. air dried Main constituents Molecular Extractable techniques is given in Table 5 [11].25 2.13 1. giving better yields and a good quality essential oil.

Table 6 E€ect of milling degree and type of extraction on the dry residue and tannins content of tincture of tormentil 4.12 2. Moreover.45 washing out (rinsing) the cell contents once the walls are Maceration 0. This e€ect could be employed as a tool were also claimed to increase the extraction yield. The alkaloid yield during the extraction of Rauwol®a by electrical discharge was increased by 25%. the contact be. Both phenomena are signi®cantly e€ected by Vortical extraction '' 5. This extraction technique is represented in Scheme 3. . In the case of low frequency sonication degradation ences between classical and vortical extraction diminish. It is worth noting increased.72 2.45 broken. according to Boiko and Mizineko [16].15 (Fig. the production of beer [18].60 ultrasonic irradiation.40 2. Ultrasonic extraction A number of papers have been published dealing with the ultrasonically assisted extraction of di€erent vegetal materials.28 physical phenomena: di€usion through the cell walls and Vortical extraction '' 5. glands (external or internal) that are ®lled with essential Scheme 3. Schematic diagram of an electrical discharge extraction unit. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 307 suggested for the ®rst time by Issaev and Mitev [14] and performed by the same authors [15] for Cytisus laburnum (broom). that when high frequency ultrasound is employed. the dynamic cavitation bubbles are produced and their extraction yield did not increase signi®cantly however collapse acts in a similar way to the e€ect of ultrasonic the degradation of the herb constituents was diminished. especially when alkaloids are Electrical discharges within the extraction mixture being extracted. It was shown that during ultrasonic ex- traction it was possible to save some 30±40% of hops in obvious that using a high speed stirrer. devices.5 mm 5.1±0. process [17]. 3. Some cells exist in the form of Rotation speed of vortex: 14. All authors working with this type of apparatus noted that during electrical discharges. tween vegetal material and solvent is improved and Several references concerning ultrasonically assisted therefore the di€usion process through the cell walls is extraction are summarized in Table 7. Extraction mechanisms Extraction method Milling degree Dry residue Tannins (%) (g) Vegetal tissue consists of cells surrounded by walls Maceration 2±5 mm 4.4. M. The extraction mechanism involves two types of Vortical extraction '' 4.000±20. Schematic diagram of a tetra¯uoroethane extraction unit. during vortical extraction hydro. If the vegetal material is well milled.75 2. One of the ®rst citations concerning ultrasonic extraction (1952) was related to hop extrac- tion in an aqueous medium and showed that ultrasonic extraction was comparable with the boiling extraction Scheme 2.000 RPM.35 Maceration Up to 1 mm 4.05 2. as to help in the extraction of medicinal compounds by using lower frequencies to assist in the degradation of toxic alkaloids during the process. the di€er. becomes more important. 1).00 2. cavitation bubbles are produced and that this technique therefore has similarities to ul- trasonic extraction.

of essential oil. For internal glands. Eugenol extracted It is obvious that reducing the size of the vegetal time (min) technique gree (g/100g) material particles will increase the number of cells di- 30 Silent not milled 4. Fig.20 to ultrasonically induced cavitation. using 1 W/cm2 [29] 800 Inula helenium and Telekia spec.308 M. Silent method involve only stirring. but decrease the glycoside yield [27] due to H2 O2 formation 20 Berberine US extraction 50% greater in 0. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 Table 7 Examples of ultrasonically assisted extraction Ultrasonic fre.64% and 0. is facilitated by soni- cation.5 h. a Extraction solvent ethyl alcohol 96%.1±0.95% US alkaloids extraction yield in 20 min.5 mm 25. No degradation of inulin. Schematic diagram of vegetal cell structures. Extracted drugs Remarks References quency (kHz) 2400 Cinchona bark No yield improvement (too high frequency US) [19] 400 Peanuts (oil) Ultrasonic yield increased when hexane is used as solvent [20] 500 Belladonna leaves Similar yield as maceration.66 should be borne in mind however that powerful soni.1±0. but 40 kHz are more e€ective [23] 20 Cinchona bark US extraction gives 15% more alkaloids in 1. compared with alkaline [28] extraction for 24 h 1000 Urtica dioica US extraction gives better results after 5 min. as well as fat oil. It 30 US 0. maceration 8 h for the same yield [22] 20±40 Datura stramonium (thorn apple) US o€er 9% greater alkaloids in 1 h.22 utilized by milling the material before extraction. oil. no decomposition of alkaloids.5 h comparing with 7 h [24] Soxhlet. Ex.26] with 0. Extraction Extraction Milling de. the cavitating solvent and consequently are readily dis- stroyed by sonication. the second to brucine.10 rectly exposed to extraction by solvent and thus exposed 30 Silent 0. 1. cation can itself serve to mill the vegetal material.2% and 0. A characteristic of such glands (when external) is ternal essential oil glands are already exposed directly to that their skin is very thin and can be very easily de. it is the milling degree of the Table 8 vegetal material which plays an important role and this In¯uence of milling degree on the extraction of clove ¯owersa is illustrated in Table 8 [32]. [31] sition a First ®gure refers to strychnine. This e€ect can be 30 US not milled 4. .94% in 8 ha 800 Digitalis leaves US lead to similar or better yield. 1000 Nux vomica seeds 1. for [21] short time sonication 25 Rauwol®a roots US time 15 min.5 mm 32. This explains why the extraction rupted. cleaning bath with stirring. good yield for shorter time (10±40 min) [30] iosa 1000 Amarantus retro¯exus 5 min sonication do not a€ect the extracted amino acids compo. compared [25.

7 27.5 '' 1 h US 18.5 31.0 22. in some cases.5 25.0 20.3 7. to obtain good extraction yields by direct or indirect Ultrasound increases the swelling index i.4 27.8 Mint Mentha piperita Classic 8.5 22. 2. An increase in the bath or probe system. una€ected (Figs.4 8.0 18.2 '' 1/2 h US 16.0 13.8 26. In both cases it is preferable to use a uptake by the vegetal material during sonication.3 Hops Humulus lupulus Classic 20.6 22. This will improve the di€usion process and therefore To perform ultrasonically assisted extraction is not enhancing mass transfer.7 4. GLYW: glycerol±water (3.2 26. ETHW: ethanol±water (70 v/v).2 Marigold Calendula ocinalis Classic 16.0 22.0 ± 16.6 15.0 9.5 4.4 ± 14.3 26. break the hypothesis for extraction improvement. 2 and bath (Figs.3 17.4 12. Using such equipment it is possible Table 9 [33].2 ETH: ethanol±water (94 v/v).3 26.2 3.5 9. .8 '' 1/2 h US 17.7 7. was found to destroy all excretion hairs as well as part of (ii) the mass transfer of soluble constituents from the the leaves. normal ultrasonic extraction devices such as a cleaning compared with mechanical stirring.0 22.5 15.3 11.2 7.0 32. WATER: water.2 21.7 Peganum harmala Classic 16.6 3.6 '' 1 h US 19. Table 9 Comparison of extractive value of sonicated and silent methods for some vegetal species [29] Vegetal species Method ETH ETHW WATER GLYW EETH Fennel Foeniculum vulgarae Classic 10. dried vegetal material is used. M. cesses. The enhancement of vegetal material swelling induced by ultrasonic treatment [29]. Ultrasound can facilitate swelling and hydration and 5.2 '' 1/2 h US 13.0 24.3 28.0 23.4 24.8 9.0 '' 1 h US 14.0 ± 15. The external oil glands (excretion (i) steeping vegetal materials in solvent to facilitate hairs) were observed and the lower frequency sonication swelling and hydration processes. may not be the only mechanistic swelling of vegetal tissue can.6 '' 1 h US 9.0 28.5 27. 6 and 7). The mechanical stirrer and to cool the extraction mixture Fig. 3±5) [33].2 19.0 30.4 28. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 309 The ultrasonic breakdown of vegetal cells using extractive value is much greater under sonication.0 31.3 26.e.0 7. whereas higher frequency left the leaf tissue material to solvent by di€usion and osmotic pro.2 13.5 21.0 29.3 '' 1 h US 27.2 16.4 16.5 v/v) and ETEH: ethyl ether.2 '' 1/2 h US 9. Laboratory and large scale ultrasonic extraction so cause an enlargement in the pores of the cell wall. the water extraction [34]. Both steps have been shown to dicult on a laboratory scale using a simple cleaning be sensitive to sonication as can be seen in Fig.5 '' 1/2 h US 22.0 30. especially when cell walls which favors the washing out process.0 6.8 31. This is because solvent The mechanical e€ect of ultrasound during extraction extraction from dried material is a two stage process has been demonstrated in the case of marigold leaves involving: when sonicated at two di€erent ultrasonic frequencies (20 and 500 kHz).

shown a high density of excretion hairs. Experimental setup for indirect extraction using a cleaning bath. large amounts of vegetal material can be employed. Pot marigold petal sonicated at 20 kHz. 8). If the same volume of solvent is used but the vegetal mass is divided into two portions the extraction can be carried out in two stages. when soft vegetal material is employed. 7. This is because the vegetal material is too concen- trated and dampens the transfer of ultrasonic energy. vegetal material can be extracted. 6. A possible industrial reactor for vegetal mass ex- traction is given (Fig. This requires a glass vessel provided with a stirrer and a cooling jacket. whereas using the direct procedure. In some cases. All excretion hairs were destroyed by ultrasound. Fig.310 M. 8. Fig. 3. horn. . 5. Experimental setup for direct extraction using an ultrasonic COPERNICUS programme (ERB-CIPA-CT94-0227. 9). Only top of excretion hairs are destroyed. 4. it is not possible to perform extractions with such a device using the normal ratio of vegetal material/solvent of 1/10 (for certain herbs this can be 1/5). Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 Fig. By indirect sonication. In the second the decanted solvent from stage 1 (containing the extract from the ®rst stage) is used. Following on from the results obtained during the research work done under an EU Fig. Pot marigold petal sonicated at 500 kHz. Experimental setup for direct extraction using a cleaning bath. Another device that could be used for ultrasonically assisted extraction is the probe system (Fig. Control: nonsonicated. since the absorption of ultrasonic energy can cause warming. Fig. only small amounts of Fig.

2. From the time when the end involved St. 11). Possible setup for an ultrasonic extraction reactor. This is obtained from a mushroom (Colletotrichum lation procedures. JohnÕs wort herb extraction in ethyl control of agriculture pests e. and Fig. producing mainly ethyl alcohol extracts for the Romanian market (Fig. The sonochemical approach will be of great bene®t to lelopathic properties. JohnÕs wort herb extraction at indus- COPERNICUS research programme started. savory on the germination of wheat seeds is shown in tract was 50% greater than that obtained classically. 10) [35]. . 1995). Brasov. involving 28 days of maceration with continuous stirring in ethyl alcohol at 45°C.g. gloeosporides) which secretes a molecule which is toxic towards vetch [37]. Better extraction yields were obtained using similar herb/alcohol mixtures under so- nication after 6 h. 6.1. over 50 trial level. working capacity) and operates in the PLAFAR factory. Natural compounds A particularly good result using the ultrasonic reac. M. isolation of compounds. New and emerging research involving sonochemical 6. One of the ®rst experiments performed to this species in the neighborhood. the targeted components also seem to be better ex. The reactor is of 1 m3 capacity (700± 850 l. at room temperature. 9. Twelve experiments with di€erent herbs were per- formed on an industrial scale using classical methods Fig. It is evident that at the correct concentration of tracted. after ology. phytopharmaceutical technology as it is used more ex- hibitory e€ect of the essential oil obtained from winter tensively for the rapid and ecient extraction of plants. hibited. Collego is used to con- alcohol where a very good yield was obtained in a much trol vetch from rice and soybean cultures in the USA. This revealed that the hypericine content of di€erent herbs and several plants have been extracted the extract reached the desired level in a much shorter and compounds isolated from them. as can be seen in the IR spectra of both extracts winter savory oil. 12 [36]. compared with the control. To illustrate such work the in. 10. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 311 Fig. from herbs have already proved to be useful for the tor involved St. Industrial ultrasonic reactor. The dry residue of the ultrasonic ex. the Romanian team designed and built the ®rst industrial ultrasonic reactor dedicated to the solvent extraction of herbs. The extraction is time than classical maceration or percolation method- simple and fast using the ultrasonic technique and. New phytopharmaceutical technology extraction In order to establish ultrasonic extraction as a new 6. Allelopathy industrial technology it is important to identify and put into place those parameters important for scale-up. each could be tested for its al. the seedling growth is completely in- (Fig. As a Allelopathy can be de®ned as the ways in which some ®rst step in this process a commercial product should be plants can use their own chemicals to control other plant identi®ed. shorter time than under classical maceration or perco.

[1] M. 1989. Academy for partial ®nancial support. Brau. Phytopharmaceutical Technology. Les Plantes dans formation presented in this paper: la Therapeutique Moderne. Ultrasonically assisted extraction is a versatile tech. Lazurca. T. E. [7] I. scale. Schmidt. 11. M. 1. 7. 12. Brinzan. Tecnologie Chimiche 1 (1996) 76. Advances in Applied Allelopathy. Ciulei. London.C. Mason.L. Hertfordshire. Vinatoru. tion and should prove to be a powerful tool for the [3] A. P. D. Vinatoru. [4] CulpeperÕs Complete Herbal.-Rundschau 1 (1953). Infrared spectra of classic and ultrasonic industrial extract. Rice. 1975. Schmall. Grigorescu. M. Pinkas. Filip.J. Stanescu. [6] An old manuscript containing a drawing of this herb can be found in the Romanian History Museum and this refers to the fact that Acknowledgements the Tracs people discovered and used it. Paris. 4 (1997) 135. Torck. G. University of Oklahoma Press. Petcu. [2] E. 1993. 1995 and SAFE COST D10/0016/99) of the research Bacneanu. Inhibitory e€ect of winter savory essential oil on wheat seedlings. Ultrason. Abstr. Stilpeanu. Ultrasound has been proven to assist solvent extrac. D. UK. 1995.312 M. Chem. P. M. Bezanger-Beauquesne. work included in this paper and to the Romanian [9] M. Medical Publishing House. Phyto- Thanks are due to EU for ®nancial support (CO. PERNICUS research program ERB-CIPA-CT94-0227- [8] M. chemistry and Phytotherapy. Biological control of weeds and plant diseases. C.I. . Vija.H. Fig. Medicinal Plants. 2. Schweiz. List. M. U. Bucha- rest. Velea. O. S. Hey- den. 47 phytopharmaceutical extraction industry. Conclusions References Two main conclusions can be drawn from the in. Wordsworth. Radu. Sonochem. M. Toma. A Book of Natural Remedies for Ancient Ills. 1995 (published for nique that can be used both on a small and large the ®rst time on 5th September 1653). (1954) 2932. Vinatoru / Ultrasonics Sonochemistry 8 (2001) 303±313 Fig. [5] P.

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