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a study of the quality of a local herbal tea and volatiles of parinari ...

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3.10 Identification <strong>of</strong> volatile constituents<br />

3.10.1 GC <strong>and</strong> GC-MS conditions for SPME<br />

The head-space <strong>volatiles</strong> were analysed by GC-MS (Agilent 6890N GC system coupled<br />

directly to a 5973 MS). The splitless injection was carried out manually at 24.79 psi <strong>and</strong><br />

an inlet temperature <strong>of</strong> 250 0 C. The GC system equipped with a HP-Innowax<br />

polyethylene glycol column (60 m x 250 µm i.d., 0.25 µm film thickness was used. The<br />

oven temperature program was 60 0 C for <strong>the</strong> first 10 min, rising to 220 0 C at a rate <strong>of</strong> 4<br />

0 C/min <strong>and</strong> held for 10 min <strong>and</strong> <strong>the</strong>n rising to 240 0 C at a rate <strong>of</strong> 1 0 C / min. Helium was<br />

used as a carrier gas at a constant flow rate <strong>of</strong> 1.2 ml/min. Spectra were obtained on<br />

electron impact at 70 eV, scanning from 35 to 550 m/z. n- Alkanes (C6-C24) were used<br />

as reference points in calculation <strong>of</strong> retention indices (RI). Component identifications<br />

were made by comparing mass spectra <strong>and</strong> retention indices. Library searches were<br />

carried out using NIST, Mass Finder, Flavour <strong>and</strong> <strong>the</strong> Baser library <strong>of</strong> essential oil<br />

constituents by comparing mass spectra <strong>and</strong> retention indices (Viljoen et al., 2008).<br />

3.10.2 GC <strong>and</strong> GC-MS conditions for hydrodistillation, s<strong>tea</strong>m distillation<br />

<strong>and</strong> CFMD samples<br />

Extracts from hydrodistillation, s<strong>tea</strong>m distillation <strong>and</strong> cold finger molecular distillation<br />

were analysed using <strong>the</strong> following conditions: A GC-MS (Agilent 6890N GC system<br />

coupled directly to a 5973 MS) was used. A volume <strong>of</strong> 1µl was injected (splitless) using<br />

an autosampler at 24.79 psi, an inlet temperature <strong>of</strong> 250 0 C. The GC system equipped with<br />

a HP-Innowax polyethylene glycol column (60 m x 250 µm i.d x 0.25 µM film thickness)<br />

was used. The ion source (electron impact ionization <strong>and</strong> <strong>the</strong> GC-MS interface<br />

temperature) was 260 0 C. The oven temperature program was 60 0 C for <strong>the</strong> first 10 min,<br />

rising to a rate <strong>of</strong> 4 0 C/min <strong>and</strong> held for 10 min <strong>and</strong> <strong>the</strong>n rising to 240 0 C at a rate <strong>of</strong><br />

53

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