Optimization of supercritical carbon dioxide extraction of essential oil from spearmint (Mentha spicata L.) leaves by using Taguchi methodology

https://doi.org/10.1016/j.supflu.2012.03.011Get rights and content

Abstract

In this study, the essential oil of aerial parts species of a plant called Spearmint was extracted by CO2 to optimize the results of the supercritical extraction process. In order to achieve maximum total yield extraction and SF-CO2 concentration, tests were done in a laboratorial pilot considering the Taguchi method under following condition: pressure. 90,100,140,170 bar, temperature. of 35, 40, 45, 50 °C, mean particles size: 250,500,710,1000 μm, flow rate 1,3,5,8 ml/s and dynamic time 30,50,90,120 min. The optimizing conditions for SCE and SF-CO2 concentration are: 90 bar, 45 °C, 500 μm, 5 ml/s, 120 min and 90 bar, 35 °C, 250 μm, 1 ml/s, 30 min. SCE total yield and CO2 concentration are 2.032% and 0.033 mg/ml. In similar and optimal conditions of extraction, supplementary tests were done so resulted and experimental amount of the calculated sum are in accordance with total yield extraction and SF-CO2 concentration. This is the first report announcing optimization of spearmint SCE by use of Taguchi method.

Highlights

► Optimization of experimental conditions of the SCE Spearmint essential oil is important. ► Determination and confirmation of optimum yield SCE of Spearmint essential oil. ► Estimate and confirmation of SC-CO2 optimum concentration in SCE process. ► This first report announcing SCE optimization by using Taguchi method. ► SCE essential oil quality higher than essence extracted by traditional methods.

Introduction

Lamiaceae family is one of the biggest herbal families that have geographical and universal dispersion. This type is grown in all around the world apart from Antarctic and northern region. These families consist of about 200 genuses and between two or 5000 species of fragrant plant and short shrubs having a large diversity [1], [2], [3]. Respectively, morphological characteristics of Lam families includes quadrangle stems, simple leaves arranged in vertical direction that have the reciprocal and alternative forms, with five-part sepal and two or four stamens ocymun bacilicum, rosmarinum officinalis, Thymus vulgaris, Origanum vulgare and Menthe belong to the same family [4].

The menthe or mentha genus, that has a vast diversity and importance, is one of the most important one in this family used by human being over 2000 years that is grown in all of 5 continents having remarkable and commercial importance. Menthe has thirteen hybrid named and composed of 19 geographical diversity [5], [6], [7]. This menthe genus has 25–30 particular species growing in Europe, Asia, and South Africa [8]. Some of the important species of this genus are Mentha spicata L., piperita L., aquatica L., pulegium L., etc. that grow in all around the world. The M. spicata L. or spearmint species or with the abbreviated name mint is the same green menthe or edible menthe that is used more frequently. Spearmint is a cross breeding species resulted from M. longifolia and rotundifolia. Menthe is one of the herbs that are so important because of its essence and pharmaceutical compounds.

Because of its benefits and economical values the menthe is one of the most important herb and many researchers have focused their attention on it in the way they can increase its yield and they can know the important factors involving the quality and the quantity of the extraction essence. The green menthe or the edible one that is the other species of this family, has more usage [7], [9], [10], [11], [12], [13].This family and this herbal species of mint is the rich source of poly phenolic compounds and, therefore have a strong antioxidant properties used in alimentation industry that prevent the oxidation. This material can be a suitable substitute for artificial and industrial antioxidants like butylated hydroxyl toluene (BHT), and butylated hydroxyl anisole(BHA). Because of the harmful effect of artificial and industrial antioxidants on human being‘s health; the natural alternative is more emphasized [14], [15], [16].

The recent studies show that the Lamiaceae is a potential resource for natural antioxidants. This property depends on some compounds such as flavonoids, diterpenes, phenolic and phenolic acid [17], [18], [19], [20], [21], [22]. The antimicrobial property of both species of menthe herbal essence has been proven and has a vast industrial, pharmaceutical, and cosmetic use and its consumption is increasing in the world [23], [24], [25], [26], [27]. The menthe is largely used in the conventional medicine because of its antispasmodic, antiseptic, and emmenagogue effects. The spearmint essential oil is used for the different kind of chewing gums, beverages, cosmetic products, perfumery, toothpastes and mouth washes [28], [29].

This valuable essence has important compounds such as carvone, Methone and d-limonene; itself is a strong insecticide and that has mutagenic activity. Also this essence has anti-fungal, antiviral, treat fever, diuretic, stimulant, and bronchitis properties, which are suitable for cramp, gastritis, headaches, indigestion, nausea and lots of other cases [22], [23], [30], [31], [32], [33].

So far different kinds of techniques have been used for the extraction of the herbal essence and the isolation of the important essence. Distillation manners, steam distillation, hydro distillation, and organic solvent extraction that consist of varied set of maceration percolations and soxhlet techniques used since long time conventionally. Conventional Sechelt extraction is a standard common technique that has a lot of problems such as long period of extraction, high consumption of chemical solvent, problem of solvent separation, toxic solvent and high cost of energy. The manners of distillation used in high temperature, are not suitable for the valuable compounds that are sensitive to temperature and can be resulted in reduction or loss of product. The supercritical extraction methods that is completely new than these methods has not the problems of earlier and conventional techniques. Because of its unique properties such as high solubility, low viscosity of supercritical fluid and fine selectivity property that present a vast use in alimentation and pharmaceutical industries and the extraction of natural and herbal raw materials [34], [35], [36], [37], [38], [39].

CO2 with critical condition C(0.47 mg/ml), T(31.18 °C), P(73.8 bar) has many interesting properties such as safety, inflammability, and inexpensiveness which like the other supercritical fluids has no free residue in product having environmentally friendly character that is highly suitable for the supercritical extraction. Despite of multiple problems and because of the simple and facility of use, the manner of extraction with solvent is common yet [40], [41]. So far the extraction of the herbal essence of M. spicata L. has been reported in conventional common manner such as distillation and the extraction with different chemical solvents and in some cases the supercritical extraction of herbal essence has been included. In some cases of the supercritical extraction, the co-solvent or modifiers (co-solvent) has been used for increasing the yield of extraction [17], [23], [25], [27], [36], [42], [43], [44], [45].

In some published articles and most review papers related to supercritical extraction of the different herbal species in which, the extraction of herbal essence of M. spicata L. has been discussed using mathematical modeling, the extraction of edible an herbal menthe has been also studied [19], [24], [45]. In some of published articles related to the supercritical extraction of this herbal species of spearmint, the design of experiment has been done and we have calculated the maximum yield of the herbal essence and the optimal condition of the extraction. In spite of the fact that researches done in this area, it seems optimization of supercritical extraction of spearmint essential oil has been performed using Taguchi testing method was not done yet and this is the first report announcing [17], [25], [27], [36]. Fig. 1 shows this valuable herbal plant.

Section snippets

Materials and method

Herbal samples of M. spicata L. were cut and collected as the aerial part and near to the period of flowering at the end of summer from the farms of south west of Iran in Kohgiluye and Buyerahmad province. The samples were very fresh and fragrant and dried in shadow along with dry weather with low moisture and have been kept in suitable container and lace before the beginning of the tests. The time of drying lasted about 2 weeks. The wet samples had more than 80 percent humidity.

Results and discussion

Based on experiments designing in the framework of Taguchi method and according to array and orthogonal L16, and considering the change of condition and different parameters such as pressure and time of extraction, supercritical flow rate, mean particles size of feed powder and dynamic time, sixteen times of test and just one repetition, we have done in sum 32 main tests. We have subsequent results in this section. The study of different parameters, similar pressure, temperature, dynamic time,

Conclusion

Applying Taguchi method for the first time, in this laboratorial research, supercritical extraction of edible spearmint herbal essence was done in order to achieve the maximum of extraction's total yield and supercritical fluid concentration. We have determined effect of five efficient parameters in the process of extraction regarding optimum conditions. The optimum conditions of extraction for the maximum yield of extraction are 2.032%: pressure of 90 bar, the temperature of 45 °C, medium size

Acknowledgment

Hereby we appreciate all those who cooperated with us at different stages of this experimental research and study, particularly library and laboratory staff of Sharif, Kashan and Shiraz University, as well as the great helps of Gachsaran Gas and Oil Production Company (GS NISOC).

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