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.
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Master
Keywords
Pharmaceutical science , Parkia Speciosa seeds
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