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Recent Extraction Techniques For Natural Products Microwave Assisted Extraction
Recent Extraction Techniques For Natural Products Microwave Assisted Extraction
In the last 10 years there has been an increased interest in using techniques involving microwave-assisted
extraction and pressurised solvent extraction in analytical laboratories. This review gives a brief overview
of both methods, and reports on their application to the extraction of natural products. The influence of
parameters such as the nature of the solvent and volume, temperature, time and particle size of the matrix is
discussed. Through numerous examples, it is demonstrated that both techniques allow reduced solvent
consumption and shorter extraction times, while the extraction yields of the analytes are equivalent to or
even higher than those obtained with conventional methods. Copyright # 2002 John Wiley & Sons, Ltd.
Keywords: Microwave-assisted extraction; solidliquid extraction; supercritical fluid extraction; pressurised solvent
extraction; accelerated solvent extraction; enhanced solvent extraction; natural products.
INTRODUCTION
A broad spectrum of solidliquid extraction (SLE)
techniques is widely used for the early purification of
natural products from plant material and micro-organisms. Classically, SLE can be divided into traditional and
recent methods. Traditional methods include Soxhlet
extraction, maceration, percolation, turbo-extraction
(high speed mixing) and sonication. These techniques
have been used for many decades; however, they are very
often time-consuming and require relatively large
quantities of polluting solvents. Supercritical fluid
extraction (SFE), microwave-assisted extraction (MAE)
and pressurised solvent extraction (PSE) are fast and
efficient unconventional extraction methods developed
for extracting analytes from solid matrixes. Numerous
review articles and textbooks have been published on
SFE (Lee and Markides, 1990; Westwood, 1993; King
and Bott, 1993) and a number are more particularly
dedicated to SFE of natural products (Castioni et al.,
1995; Smith, 1995, 1996; Jarvis and Morgan, 1997). The
present review deals with the application of MAE and
PSE to the extraction of secondary metabolites from plant
material.
MICROWAVE-ASSISTED EXTRACTION
Microwaves have been used since World War II
following the development of radar technology, and later
the first commercial application of microwaves concerned domestic ovens. The use of microwave energy as
* Correspondence to: P. Christen, University of Geneva, School of Pharmacy,
Laboratory of Pharmaceutical Analytical Chemistry, 20 bd dYvoy, CH-1211
Geneva 4, Switzerland.
Email: philippe.christen@pharm.unige.ch
106
Dielectric constant
(20C)
Dipole moment
(25C) (Debye)
1.89
2.4
8.9
20.7
24.3
32.6
78.5
<0.1
0.36
1.14
2.69
1.69
2.87
1.87
MICROWAVE-ASSISTED EXTRACTION
107
108
Matrix
System
Extraction conditions
Reference
Vicine, convicine
(pyrimidine glycosides)
Domestic oven
Gossypol
Cotton seeds
Domestic oven
Sparteine (alkaloid)
Lupine seeds
Domestic oven
Terpenes (linalool,
terpineol, citronellol,
nerol and geraniol)
Essential oils
Closed vessels
Monarda stulosa,
Allium sp.
Mentha piperita, Thuja
occidentalis
Rosemary and
peppermint leaves
Modied domestic
oven
Modied domestic
oven
Domestic oven
Methanol:water (1:1);
two successive
irradiations (30 s) with
an intermediate cooling
step
Three cycles of
irradiation (30 s) with
cooling steps in
between
Four cycles (30 s) with
cooling steps in
between
10 mL
dichloromethane;
475 W; 10 min; 90C
Hexane
Domestic oven
Domestic oven
Carotenoids
Plant leaves
Fresh leaves of Lippia
sidoides
Paprika powder
Taxanes (paclitaxel)
Closed vessels
Ergosterol
Withanolides
Fungal contaminations
Iochroma gesnerioides
leaves
Domestic oven
Open cell, focused
Cocaine and
benzoylecgonine
Alkaloids
Erythroxylum coca
leaves
Senecio sp.
Closed vessels
65100C
Volatile oils
Essential oils
Essential oils
Essential oils
Closed vessels
Hexane, alkanes
(transparent solvents)
Hexane, carbon
tetrachloride, toluene;
750 W; <60 s
Hexane; <60 s
High cooking level; 5
min
50 W; 120 s; <60C
MICROWAVE-ASSISTED EXTRACTION
109
Open vessels
Very few papers have been published concerning the
focused microwave extraction of natural products.
Alkaloids. Cocaine and benzoylecgonine were extracted
from coca leaves (100 mg) by focused MAE (Brachet et
al., 2002). The extraction was optimised by taking into
account several parameters such as the nature of the
extracting solvent, particle size distribution, sample
moisture, applied microwave power and radiation time.
MAE was found to generate similar extracts to those
obtained by conventional SLE but in a more efficient
manner. Indeed, 30 s were sufficient to extract cocaine
quantitatively from leaves, using methanol as solvent and
a microwave power of 125 W.
Copyright # 2002 John Wiley & Sons, Ltd.
110
MICROWAVE-ASSISTED EXTRACTION
111
Matrix
Taxanes (paclitaxel,
baccatin III and 10deacetylbaccatin III)
Naphthodianthrones
(hypericin)
ASE
ASE
Naphthodianthrones
ASE
Saponins
ASE
Terpenes
Thyme (Thymus
vulgaris)
ASE
Flavonolignans
ASE
Curcuminoids
Turmeric rhizome
(Curcuma
xanthorrhiza)
Osage orange tree
(bark) (Maclura
pomifera)
Erythroxylum coca
leaves
Iochroma
gesnerioides leaves
ASE
ASE
PSE
PSE
Reference
112
CONCLUSIONS
MAE and PSE are emerging as attractive alternatives to
conventional extraction methods such as Soxhlet,
percolation, digestion, extraction under reflux, sonication
and in some cases steam distillation. Initially employed
as a digestion method for different sample types such as
environmental, biological and geological matrixes, MAE
is now widely accepted in analytical laboratories. The
main advantage of MAE resides in the performance of the
heating source. The high temperatures reached by
microwave heating reduces dramatically both the extraction time and the volume of solvent required. PSE works
according to the principle of SLE with elevated
temperature and high pressures in order to keep the
solvent in a liquid state. Enhanced diffusivity of the
solvents leads to an increase in extraction speed and
efficiency. With both MAE and PSE, recoveries of
analytes and reproducibilities are improved and, therefore, both methods should be considered as interesting
alternatives with the limitation that experimental conditions must be chosen in order to avoid possible thermal
degradation. Finally the costs of the specialised equipment (especially PSE) may also influence the choice of
the extraction technique (Camel, 2001).
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MICROWAVE-ASSISTED EXTRACTION
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