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Scientific Publication

Elena Stashenko 1) Jairo René Martínez, Carlos Macku, and Takayuki Shibamoto 2)
1) Department of chemistry, Universidad Industrial de Santander. A.A 6678, Bucaramanga. Columbia.
2) Department of Environmental Toxicology. University of California, Davis, California 95916, USA

Key Words:

Summary

1 Introduction

2 Materials and Methods

2.1. Essential Oil Extraction

Ilang Ilang flowers were gathered in Bucaramanga Santander (Colombia) during May 1991. Recently collected, mature, yellow flowers of ylang-ylang (A) their petals © and ovanes (D) and whole flowers collected 24 hours before the distillation (B) constituted the starting material Steam distillation was carried out by passing steam through a 5 liter round-buttoned flask containing plant material and collecting the condense (water and oil) in a flask with sodium chloride.

The condensate was extracted with ethylether. Sodium sulfate was added to remove moisture and the solvent was then separated by rotary evaporation 800-1000 g of each type of material was subjected to steam distillation to afford essential oil samples IA. IB, and IC (1h extraction), and IIA, IIB, IIC, and D (2h extraction). The yields were under 0 55% for 1 hour of extraction and 1.05% for 2 hours of extraction. The lowest yield corresponded to the extraction from flower ovaries. 0 05% and 0 35% for 1 and 2 hours of distillation, respectively The essential oil contents reported are averages of three extractions.

2.2. Essential Oil Analysis

HRGC analysis of the samples was performed on a Hewlett Packard (HP) 5890-II-gas chromatograph equipped with a flame ionization detector and a HP 3396 A integrator. The columns used were an HP 20M (used silica capillary column (50 m. 0.2 mm id), coated with Carbowax 20M (0.20 urn phase thickness) and a DB-1 (j&W Scientific, Folsom, CA) cross-linked fused silica capillary column (30 m, 0.25 mm i d) coated with dimethyl polixilosane (0.20 pm phase thickness) The oven temperature was programmed from 50 º C (5 min hold) at 25 º C min -1 to 180 º C (hold 20 min) for the HP 20m column and from 50 º C (5 min hold) to 200 º C (15 min hold) at 35ºC min -1 for the DB -1 column. The helium inlet pressure was 195 kpa and 78 Kpa, whit velocities of 19 cin s -1 (split 20 ml nun -1) and 20 cms -1(Split 50 ml min-1) for the HP 20M and DB-1 columns respectively In all runs, the detector and injector temperature were set at 250 º C. The injection volume was 0.2 pL of a 30 v/v solution of ylang-ylang oil in dichloromethane.

A HP 5890 gas chromatograph interfaced to a VG Trio ll mass spectrometer with a VG 11-250 computer data system was used for MS identification of the GC components. The column and oven conditions used were as described above. The temperature of the ionization chamber and of the separator was 220ºC, the energy of the ionizing electrons was 70 eve the cathode emission current was 300 ma and the accelerating voltage 3V Mass spectra and reconstructed chromatograms were obtained by automatic scanning in the 30-350 m/2 range at 2-second intervals Chromatographic peaks were checked

for homogeneity with aid of the mass chromatograms for the characteristic fragment ions A JEOL EX-90 FT NMR spectrometer was used for the 1H and 13C analysis of the oils dissolved in CDCL infrared spectra were obtained a Perkin Elmer 1750 FT-IR spectrometer.

3. Results and Discussion

Figure 1.

Typical gas chromatogram of Ilang-Ilang essential oil from Colombia (sample IA) (j&W Scientific. Folsom, CA) cross linked fused silica capillary column (30m, 0,25 mm i.d.) coated with dimethyl polysiloxane (0,20, um phase thickness): column temperature programmed from 50°C (5 min hold) to 200 °C (15 min hold) at 3.5 /min carrier gas helium, 78 Pa, split 50 ml/ min. See table 1 for peak identification.

It is worth noting that the 30 m DB 1 column was able to resolve all the oil components. Thus the time consuming runs associated with the use of longer (60 - 100 m) capillary GC columns can be avoided in the analysis of Ylang - Ylang oils.

An asterisk under the 13C NMR and IR columns. Table 1 indicates that a characteristic spectroscopy feature was found a particular component. These feature are being collected to be tested as potential quality descriptors, in order to alternate to GC and GC-MS analysis in the routine estimation of essential quality At 90 MHz proton NMR spectra were not sufficiently resolved to permit the identification of individual components but proved to be a quick, quantitative method to determine average structural parameters of thee oil sample, such as the percentages of aromatic olefinic, and saturated hydrogens.

The 13 C-NMR peaks were assigned based on reported individual spectra (8,9) 13 out of the 16 compounds used for oil quality assessment were distinguishable in the 13 C-NMR spectrum. Relative concentrations in agreement with these calculated from the GC peak area were obtained using NOE-enhanced 13 C-NMR signal intensities corresponding to carbons of equal protonation level (10).

In figures 2 and 3, the results from table 1 were grouped into compound families in order to appreciate the effect of the variables under study. The essential oils obtained from fresh flowers contained from 1.5 to 3 times more monoterpenes and light-oxigenated compounds than oils distilled 24 hours after the flowers had been collected. The relative amount of aromatic oxygenated compounds (r- methyl-anisol, methyl benzoate, ethyl benzoate, benzyl acetate), monoterpeneols, linalool, a-terpineol, geraniol (and their acetates, was three times higher in the oils extracted from fresh flowers. Linalool was notably high in the latter *Table 1(, making them the preferred source for high quality oil. The contents of sesquiterpenes, sesquiterpeneols, and sesquiteerpenyl acetates, increased by more than 30% in the oils extracted from dry flowers. This trend was observed for different extraction times. The rapid metabolic transformations that take place as the flower dries are as strong argument in favor of locating the oil extraction facilities close to the plantations. No gains in oil quality are obtained by processing part of the flower separately. On changing from petals to ovaries, the monoterpene and sesquiterpenes contents increase, while the light and heavy oxygenated compounds decrease. The oil extracted form fresh flowers by steam distillation for one-hour places it among the so-called Extra Grade oils (1-3).

4. Conclusions

The essential oil from Colombian ylang ylang flowers contains volatile metabolites such as anethol and camphene which have not been identified in oils of other origins. Linalool, a component which appears in higher concentrations as the oil grade improves, is present in Colombian oils in concentrations more than twice the reported values for first grade oils from the Comoro Islands.

Among the composition-determining variables studied the extraction time and the flower condition were found to posses the largest influence on n the quality of the essential oil. Extra grade essential oil from Colombian Ylang Ylang can be obtained from fresh flowers using steam distillation for one hour. Medium Length (30 ml) capillary columns can be successfully used in the analysis of ylang ylang essential oils.

Acknowledgments

References

444                Vol. 16, July 1993                Journal of High Resolution chromatography