Comparative analysis of the oil and supercritical CO2 extract of Artemisia sieberi

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Abstract

Essential oils of aerial parts of Artemisia sieberi obtained by hydrodistillation and supercritical carbon dioxide extracts obtained under different conditions were compared with regard to their major components. The supercritical fluid extraction (SFE) experiments were carried out in the pressure range of 10.1–30.4 MPa, the temperature range of 308–338 K, the dynamic extraction time of 15–35 min, and modifier volume of 0–500 μl. An experimental design was carried out to map the effects of different parameters on the extraction yield of the active components and to determine the optimal conditions for the extraction of camphor from A. sieberi using SFE. The optimization of supercritical fluid extraction conditions has been carried out by Taguchi method using a three level orthogonal array design with an OA9 (34) matrix. Based on direct observation analysis, the highest yields for SFE were obtained at a pressure of 30.4 MPa, a temperature of 318 K, a dynamic extraction time of 25 min and in the absence of methanol as modifier. On the other hand, under these same conditions except a slightly higher temperature of 328 K extraction was more selective for the extraction of camphor. The chemical compositions of the SFE extract were identified by GC–MS and determined by GC–FID and then, compared with the essential oils obtained by hydrodistillation. The major compounds of oil obtained by hydrodistillation were camphor (54.7%), camphene (11.8%), 1,8-cineol (9.9%), β-thujone (5.7%) and α-pinene (2.5%). However, by using the supercritical carbon dioxide in optimum conditions, only two components represented more than 80% of the extract. The oil yield, based on the hydrodistillation was 1.7%, and the extracts of desired analytes based on the SFE varied in the range of 1.6–14.0% W/W under different conditions. The Chemical analysis revealed that components extracted under different SFE conditions possessed widely different percentage of constituents. The results indicated that by using the suitable extraction conditions, SFE is more selective than the conventional hydrodistillation method in the extraction of essential oil and the preservation of its quality.

Introduction

The genus Artemisia, with the common Persian name of ‘dermane’ and also with common English name of ‘wormwood’ includes 34 species that are found wild all over Iran (Mozaffarian, 1996). Plants are the major food sources for human beings. More than 160 individual flavonoid components have been isolated in the genus Artemisia and about one third of them are derivatives of the flavones luteolin and apigenin (Belenovskaja, 1996, chap. 18). Flavonoid components of 130 species of Artemisia have been used for the solution of taxonomic problems at the intrageneric level. Artemisia sieberi (A. sieberi) is an endemic species of Iran, which grows in many regions of Iran. This plant has several therapeutic effects on different conditions such as digestive, fungicidal growth, etc. also; it has pesticide characteristics, especially, against larvae of Anopheles insect. Camphor is a major component that is extracted from A. sieberi.

An “essential oil” can be defined as the volatile material present in plants (Reverchon, 1997, Encyclopedia of food science and technology, 1992) and is usually isolated by either hydrodistillation or solvent extraction. Hydrodistillation has traditionally been applied for essential oil recovery from plant materials. This technique has several disadvantages such as: low yield, long distillation time, losses of volatile compounds as well elevated temperatures and water which can cause the degradation or chemical modification of essential oils (Assis et al., 2000, Doneanu and Anitescu, 1998, Illes et al., 2000, Lehotay, 1997, Oszagyan et al., 1996). Also, there are a few adjustable parameters for hydrodistillation, steam distillation and solvent extraction to control the selectivity of the process. Therefore, developing attractive extraction techniques with better selectivity and efficiency are highly desirable. Consequently, the supercritical fluid extraction technique for solid materials was introduced and extensively studied for the separation of active compounds from herbs and other plants (Lang & Wai, 2001).

The supercritical fluid extraction (SFE) is a good technique for the production of flavors and fragrances from natural materials and can constitute a valid alternative to the conventional essential oil extraction methods (Caredda, Maringiu, Porcedda, & Soro, 2002). It has been widely accepted by many investigators that compared favorably with hydrodistillation the SFE provides a rapid and quantitative method for extracting essential oils from aromatic plants (Hawthorne et al., 1993, Kerrola, 1995, Stahl et al., 1988). By operating SFE in an optimal region, the pressure and temperature can be used to regulate the density; which regulates the solvent power of a supercritical fluid. Recently some articles dealing with comparative analysis of the oil and supercritical CO2 extracts of plants have appeared in the literature (Anitescu et al., 1997, Omidbaigi et al., 2003, Pino et al., 1999, Reis-Vasco et al., 1999, Sarrazin et al., 2000).

The aim of the present method was the investigating of the effects of experimental parameters such as pressure, temperature, modifier volume and dynamic extraction time on the extraction yield and selectivity of A. sieberi extracts obtained by the SFE. The effects of experimental parameters on the extraction yield and selectivity using an OA9 (34) orthogonal array were investigated. The steam distillation of A. sieberi essential oil has been studied previously (Sefidkon, Jalili, & Mirhaji, 2002). However, to the best of our knowledge no report has yet appeared on the SFE of A. sieberi.

Section snippets

Plant material

A. sieberi was collected from the southern part of Tehran (Iran) in November 2004. The dried plant was stored in a dark place. The sample was ground in a blender to produce a fine powder. The average of particle size was 0.4 mm. A voucher specimen was deposited in the herbarium of the Faculty of Pharmacy, Tehran Medical Sciences University (Tehran, Iran).

Reagents

HPLC grade dichloromethane and methanol were purchased from Aldrich. Carbon dioxide with the purity of 99.99% was obtained from Daga Company

General

In this study, we tested a static-dynamic SFE approach for yield and extraction of A. sieberi essential oil. The efficiency and selectivity were compared with those of the essential oil composition obtained by hydrodistillation. A 15 min static extraction period was employed in order to increase the sample-extraction contact duration. After 15 min of static extraction, each vessel was flushed with the supercritical CO2 for different dynamic time.

The optimization of the experimental conditions

Several parameters have to be optimized in order to

Conclusions

The extract obtained by the SFE of A. sieberi showed some differences in comparison with the oil obtained by the hydrodistillation. Statistical analysis showed that the pressure of the supercritical CO2 had a significant effect (p > 95%) on the extraction yield. Also, the selectivity of the SFE was higher than that of the hydrodistillation method. On the other hand, the SFE method offers important advantages over hydrodistillation, namely: shorter extraction time (30 min against 3–4 h for

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