ACCELERATED SOLVENT EXTRACTION:

h o ,.
m osTi AN INNOVATIVE SAMPLE EXTRACTION iUKLEAR
A L A Y S I A
KEM EN TERIAN SAIN S, TE KN O LO G I DAN INOVASI
MINISTRY OF SCIENCE. TECHNOLOGY AND INNOVATION TECHNIQUE FOR NATURAL PRODUCTS •■ X P
H. Ahm ad Hassali. A.H. AbdAziz, R. Razali,F. M ohd Saaya,B. Yaacob, N. A. M arsidi,Z.A dam and S.Khamis
M edical Technology Division, Malaysian Nuclear Agency, 43000 Kajang, Selangor, M alaysia

ABSTRACT
Accelerated solvent extraction (ASE) is one of the novel techniques that have been developed for the extraction of phytochemicals from plants in order to
shorten the extraction time, decrease the solvent consumption, increase the extraction yield and enhance the quality of extracts. This technique combines
elevated temperatures and pressure with liquid solvents. This paper gives a brief overview of accelerated solvent extraction technique for sample preparation
and its application to the extraction of natural products. Through practical examples, the effects of operational parameters such as temperature, volume of
solvent used, extraction time and extraction yields on the performance of A SE are discussed. It is demonstrated that ASE technique allows reduced solvent
consumption and shorter extraction time, while the extraction yields are even higher than those obtained with conventional methods.

INTRODUCTION A cce le rate d So lvent Extractio n (A S E ) S y s t e m .......

y Automated extraction technique that uses liquid
Medicinal plants contain curative bioactive compounds which have proven to solvents and solvent mixtures
be valuable as primary o r supplementary therapies when applied carefully y Extracts solid o r semisolid samples
(Chang et al, 2008). Th e phytochemical investigation of a plant may involve y Uses elevated temperature (40-200 °C) and
following steps: authentication and extraction of the plant material, pressure ( 1500 psi)

separation and isolation of the constituents of interest, characterization of y Elevated temperature and pressure accelerate
the extraction process
the isolated compounds and quantitative evaluation (Evans, 2008). Extraction
y Requires small quantities of solvent in short
method plays a vital role in separation and characterization of different
periods of time
phytochemicals from herbs, and screening plant extracts for novel leads. ■ ASE: 15 mL and 15 min fo r 10-g samples
Accelerated solvent extraction have been developed for the extraction of ■ Soxhlet: 8-48 h and 300-500 mL
phytochemicals from plants in order to shorten the extraction time, ■ Sonication: 1-2 hours and 200-500 mL Figu re I: A S E System
decrease the solvent consumption, increase the extraction yield, and enhance • Supports a wide range of sample sizes (mg-100 g)
the quality of extracts (Wang & Weller, 2006). • Can be used to prepare samples fo r GC, GC-MS, HPLC,LC-MS,gravimetric methods,
1C, and IC-MS analytical methods
OBJECTIVE
RESULTS & DISCUSSION
To evaluate accelerated solvent extraction technique for sample preparation
and its application to the extraction of natural products Table 2: Effect of temperature on F. deltoidea

MATERIALS & METHODS T e m p e ra tu r e P e rc e n ta g e Y ie ld

4 0 °C 18 .87 %

6 0 °C 2 1 .1 0 %

8 0 °C 2 3 .1 9 %

1 0 0 °C 2 5 .7 2 %
Figure 5: W a ter extracts of F.deltoideo le a f samples
using ASE at variable temperature________________

------ ------------ •(! n-u-utOMiCiui

.. ----- MT’.CK 'W5S1KX! M-xmtCMSCiJJi Based on UHPLC profiling
shown in Figure 6, the
results demonstrated that
there were no changes in
phytochemicals distribution
of F. deltoidea extracts
suggesting that no thermal
degradation was observed
for F.deltoidea extracts at
Table I : ASE conditions fo r F. deltoidea water temperatures as high as
extraction procedure 100 °C with the ASE
method under optimized
Parameter Condition conditions.

Solvent Water Figure 6: UHPLC chromatogram showing the profiling of phytochemicals in

Temperature 100°c F. deltoidea water extracts at variable temperature applied in ASE

Pressure 1500 Psi Table 3: Comparison of ASE technique to conventional method in the extraction of F.deltoidea
Heating 4 Minutes A c c e le ra te d S o lv e n t C o n v e n tio n a l M e th o d
P a ra m e te r
Static Time 5 Minutes E x tra c tio n a t 100°C (D e c o c tio n te c h n iq u e )
T im e 20 minutes 3 hours
Static Cycles 2
S o lv e n t C o n s u m p tio n 150 mL 573 mL
Rinse Volume 60% S a m p le w e ig h t 1602 g 57.3g
Purge Time 90 Seconds E x tr a c t w e ig h t 4.12 7.27 g

Figure 3: ASE System in Phytochemistry Cell Size 100 mL P e rc e n t Y ie ld 25.72% 12.69%

Laboratory, Malaysian Nuclear Agency Total Time 17 Minutes

f A t elevated temperature. High pressure........
y Higher analyte solubility > forces solvent into pores that are blocked
y Helps overcome matrix effects at low pressure
i~J CJI. AJ
y Viscosity of solvent is lowered y Pressure needed to keep solvents liquid at
Cell loading
u
Solvent
y
Solvent
y
Solvent
y Analytes diffuse into solvent more quickly
>
high temperatures
Cells fill faster with high pressures

c
Fill, heat, (min) dynamic
equilibrate 5 to 9 extraction
CONCLUSION
Static extraction 0-99 static extraction Accelerated solvent extraction (ASE) is an innovative sample preparation
4 cycle
technique that combines elevated temperatures and pressures with liquid

c
f
Rinse with
fresh solvent
0.5 y solvents to achieve fast and efficient extraction process. W ith proper
sample preparation and optimization of extraction parameters, nearly any

5
y
sample currently extracted with a liquid solvent can be performed in less
Purge with 1-2 time and with smaller quantities of solvent using accelerated solvent
nitrogen Static Valve
extraction.
r
Extract Total (m in )1 Jl. REFERENCES
ready 12-20 Collection Bottle
Chang,Y.S.,Mazurah,M.P.and NikM usaadah M.,(2008). Plant Health and Man - Past, Present and Future. Selangor: Forest Research
Institute. 342
Evans,W.C. 2002. General methods associated w ith the phytochemical investigation o f herbal products. InTrease and Evans
Figure 4: Process Schematic in ASE Pharmacognosy (15 ed.),N ew D elhi:$aunders (Elsevier), pp. 137-148
Wang, L.and W e ller,C .L.,(2006). RecentAdvances in Extraction o f Nutraceuticals from Plants.Trends in Food Science &Technology.
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