Development of identification technique by ftir-pca for supercritically extracted metabolites from Parkia Speciosa (HASSK) seeds
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Date
2007
Authors
Salman, Zhari
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Abstract
The qualitative and quantitative analysis on the yield of Parkia speciosa
seeds extracted by Supercritical Carbon Dioxide Extraction (SC-CO2 extraction)
were performed under various extraction conditions. The combined conditions
were interactions of temperatures at 313 K, 323 K, 333 K, 343 K, 353 K and
363 K and pressures at 20.68 MPa, 27.58 MPa, 34.47 MPa, 41.37 MPa, 48.26
MPa and 55.16 MPa. Extraction time and particle size were fixed to 50 minutes
and 250 - 300 μm respectively. An interesting behavior was found where at low
pressure, extracted yield decreased with increasing temperature while at high
pressure, the extracted yield increased with increasing temperature. This
behavior known as the retrograde vaporization was further studied by
examining the extractability values of SF extracted samples. The highest
extractability value of Parkia speciosa in CO2 was 0.458 g yield/100 g CO2 at
the interaction condition of 34.47 MPa/363 K.
A rapid identification, classification and discrimination tools using Fourier
Transform Infrared (FTIR) spectroscopy combined with chemometrics analysis
was applied to determine the profile of SF extracts in each extraction
conditions. Principal Component Analysis (PCA) was applied to the FTIR
spectra for further analysis of metabolites. Scores and loadings plot show that
this metabolomics method is suitable for the analysis of SF extracted samples
from natural products. The results obtained by this method successfully discriminate samples with high concentration of unsaturated carboxylic acid
from other samples.
The analysis of compound by Gas Chromatography-Time of Flight Mass
Spectrometry (GC/TOF-MS) was done based on percentage of similarity and
peak area of more than 75 % and 0.3 % respectively. Thiodipropionoic acid,
didodecyl ester was present with highest percentage area in most sample
conditions. Other main compounds were linoleic acid chloride, palmitic acid,
linoleic acid, myristic acid, arachidonic acid and undecanoic acid. Terpenoids
compound of β-sitosterol, campesterol and stigmasterols were identified at all
conditions, while some other compounds such as squalene and lupeol were
identified only at certain condition. The combination in chromatographic
separation with an identification technique as in GC/TOF-MS has made it
possible to detect the variability obtained by different SC-CO2 extraction
condition and separation of different chemical compounds in Parkia speciosa
seeds.
Verification of results from FTIR-PCA methods by GC/TOF-MS
successfully identified the unsaturated carboxylic acids with the highest
percentage area at conditions discriminated by FTIR-PCA methods.
Description
Master
Keywords
Pharmaceutical science , Parkia Speciosa seeds