Brazilian Journal of Analytical Chemistry - BRJAC - Brazilian Journal ...

Br J Anal Chem 2011, 03, 164–168
dE t E r m i n a t i o n o f volatilE o rg a n iC C o m P o u n d s PrEsEnt
in fruit f ro m thE gE o n o m a g a m i o v a a n d gE o n o m a
PauCiflora Palm trEEs u s i n g thE sPmE t E C h n i q uE
ra f a E l a olivEira ara u J o a , Cl a u d i o au g u s t o ollEr d o nasCimEnto a , ma r i a an i t a mEndEs a *
A) University of São Paulo, Poli- Department of Chemical Engineering, CEPEMA, São Paulo, Brazil - 05508-900
*Corresponding author:
Phone (11) 3091 2262
Email address:
anita@pqi.ep.usp.br
aBstraCt
The purpose of this study was to collect and identify the greatest possible number of
volatile organic compounds produced in the inflorescence of the Geonoma gamiova
and Geonoma pauciflora palm trees, which are plant species endemic to the Atlantic
rain forest in the Cubatão region. Sample collection and pre-concentration were carried
out using the SPME technique and compounds were analyzed by GC-MS. The samples
were extracted via the HS-SPME method using a 100 µm PDMS-coated fiber mounted
in a manual syringe holder at 30 o C for 30 min. The analyses were performed in fullscan
mode with a mass range of m/z 40 to m/z 500. The compounds were ionized
in the electron ionization ion source and separated by an ion trap mass analyzer. By
analyzing the results, we can observe that the fruit from the Geonoma gamiova palm
features 20 different volatile compounds, which were extracted and identified by the
aforementioned techniques, while the Geonoma pauciflora palm featured 15 different
volatile compounds, which were also extracted and identified. Both palms proved to
have five volatile compounds in common: 1,2-benzenedicarboxylic acid, n-capric acid
n-heptyl ester, 3,5-bis(1,1-dimethylethyl)-phenol, 2-hexyl-1-octanol.
kE y w o r d s : SPME, volatile organic compounds, GC-MS, Palm tree
in t ro d u C t i o n
Headspace solid-phase micro-extraction (HS-SPME)
is an efficient technique for the extraction of volatile
compounds from plants. HS-SPME has also been
successfully used for screening complex volatile mixtures
and for complementing information obtained from
other methods of extraction, due mainly to its simplicity
and reliability (1).
Sample preparation for the analysis of flavors and
fragrances normally involves the use of headspace, purge
and trap, liquid-liquid extraction, solid phase extraction
or simultaneous extraction and distillation techniques,
in order to concentrate the analyte in question. These
methods have several drawbacks, including a lengthy
sample preparation time and excessive use of solvents.
Solid-phase micro extraction (SPME) is a sorption and
desorption technique, developed by researchers at
the University of Waterloo (Ontario, Canada), which
eliminates most of the disadvantages pertaining to
sample preparation. (2-5).
The SPME technique requires no solvents or complex
apparatus and it can be used to concentrate volatile
and non-volatile compounds from liquid samples or
headspace, providing linear results over a wide range
of concentrations (sometimes in parts per trillion) and it
can be used with gas chromatography systems coupled
to mass spectrometry (1).
The volatile and semi-volatile compounds produced
by plants and other living entities are collectively known
as biogenic volatile organic compounds (BVOC). They
include a large number of organic substances, including
isoprene and terpenoid compounds, alkanes, alkenes,
carbonyl compounds, alcohols and esters, and they are
typically present in the atmosphere in concentrations
ranging from parts per trillion (ppt) to parts per billion
(ppb). Determining the quantity of BVOC released from
living plants is usually carried out by placing whole
plants or parts thereof in a chamber made of glass or
plastic, from which the organic compounds emitted
are collected and analyzed chromatographically. The
overall process has several drawbacks; for example,
material used for extraction may introduce artifacts
into the extracted material, the solvent used to extract
the adsorbed material can mask the detection of
compounds with low boiling points, and long sampling
periods may be necessary to capture sufficient amounts
of analyte for analysis (6).
To date, poly(dimethylsiloxane) (PDMS) coating is one
of the most widely used coatings for extracting volatile
164 Br J Anal Chem