Study of the Essential Oil Composition of Cumin Seeds by an Amino Ethyl-Functionalized Nanoporous SPME Fiber

Chromatographia (Impact Factor: 1.41). 10/2009; 70(7):1147-1151. DOI: 10.1365/s10337-009-1269-7


An ultrasound assisted SPME method with a new nanoporous SBA-15 fiber functionalized with 3-[bis(2-hydroxyethyl)amino]propyl-triethoxysilane
was successfully applied to the study of the essential oil composition of cumin (Cuminum cyminum L.) seeds. The sample was irradiated by ultrasound radiation and its volatile components were collected by the fiber from
the sample headspace and directly injected into a GC-MS injection port for analysis. A simplex method was used for optimization
of four different parameters affecting the efficiency of the extraction. Under the optimized conditions (i.e. sample weight,
0.6g; temperature, 70°C; sonication time, 12min and extraction time, 28min), the number of components identified by the
proposed method and their amounts were identical to those of a hydrodistillation technique. The extraction efficiency of the
SBA-15 fiber was superior to a PDMS commercial fiber. The major components identified were p-menta-1,3-dien-7-al, cuminaldehyde, γ-terpinene and p-cymene, respectively. The proposed method was applied to a comparative study of the essential oil composition of cumin in
three different climate conditions of the Lorestan province in Iran. The results indicated that the essential oils in the
temperate and tropical locations were 94.0 and 85.6% of the cold region, respectively.

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    • "Therefore, the development of simple, rapid and solvent-free methods for the analysis of essential oils is highly desirable. Headspace solid-phase microextraction (HS-SPME) is a relatively new sampling and concentration technique for the extraction of plant essential oils (Cao et al., 2006; Kwon et al., 2006; Lopez et al., 2006; Theodoridis 2006; Zahradnickova and Bouman, 2006; Hashemi et al., 2009b). The HS-SPME technique followed by gas chromatography–mass spectrometry (GC–MS) has proven to be a simple, sensitive and solvent-free method for the analysis of essential oil components. "
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    ABSTRACT: High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale was successfully used in isolation and purification of cuminaldehyde and p-menta-1,4-dien-7-al from the essential oil of Cuminum cyminum L. by using a two-phase solvent system composed of n-hexane-methanol-water (5:4:1, v/v/v). The targeted compounds were isolated, collected, purified by HSCCC in the head-tail mode, and then analyzed by gas chromatography (GC). A total of 12.72 ± 0.22 mg of cuminaldehyde and 10.61 ± 0.27 mg of p-menta-1,4-dien-7-al were obtained from 50 mg of the essential oil of C. cyminum L. in less than 6 h, with purities of 95.42% and 97.21%, respectively. In addition to GC-EI/MS, the identity of the cuminaldehyde was further confirmed with the retention time using the method of standard addition, while, the structural identification of p-menta-1,4-dien-7-al was performed with GC-EI/MS, (1)H NMR and (1)H-(1)H COSY.
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