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2. ENVIRONMENTAL ChEMISTRy & TEChNOLOGy 2.1. Lectures

2. ENVIRONMENTAL ChEMISTRy & TEChNOLOGy 2.1. Lectures

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Chem. Listy, 102, s265–s1311 (2008) Environmental Chemistry & Technology<br />

Table I<br />

RSD in determination of analytes<br />

Analyte RSD Analyte RSD<br />

α-pinene 13 menthone 32<br />

camphene 11 borneol 18<br />

sabinene 14 estragol 28<br />

β-pinene 9 α-cubebene 12<br />

β-myrcene 7 thymol acetáte 38<br />

α-phellandrene 10 ylangene 31<br />

3-carene 7 copaene 27<br />

α-terpinene 7 α-bourbonene 34<br />

2-nitro-p-cymene 3 isocaryophyllene 35<br />

limonene 23 β-caryophyllen 26<br />

eucalyptol 8 humulene 31<br />

γ-terpinene 4 α-caryophyllen 36<br />

β-terpineol, cis- 15 isoledene 32<br />

linalool 13 α-muurolene 36<br />

thujone 22 epizonarene 36<br />

camphor 12 karyophyllene oxide 34<br />

were as follows: the duration of sorption was 15 minutes at<br />

a temperature of 30 °C. This temperature was also used for<br />

sample conditioning. Fig. <strong>2.</strong> shows the comparison between<br />

the different durations of sample conditioning (0; 5; 10; 15;<br />

20 minutes) and it is seen that the 5-minute conditioning is<br />

the most suitable as it gives the highest response for the majority<br />

of target analytes.<br />

The repeatability of the method was determined based<br />

on 5 repetitions and is expressed as a relative standard devi-<br />

s462<br />

ation (Table I). Terpenes are listed in the table according to<br />

their increasing molecular weight. It follows from the results<br />

that lower-molecular-weight terpenes have better repeatability<br />

than more volatile terpenes with higher molecular weight.<br />

Standard deviations vary in a rather wide range of 28–38 %<br />

for substances with higher molecular weight which may be<br />

attributed to the optimization of the SPME method where<br />

some parameters (particularly the duration and temperature<br />

of sorption) were chosen at such levels to match for the whole<br />

group of 32 monitored substances.<br />

Conclusions<br />

SPME conditions used for optimalization of head-space<br />

method were follows: 15 min exposition of PDMS-DVB<br />

(65 µm) fiber at 30 °C in head-space above 0.5 g of spice<br />

sample in vial. The incubation of sample was 5 minutes at<br />

extraction temperature 30 °C.<br />

This work has been supported by by the grants given by<br />

Ministry of Education, Youth and Sports of the Czech Republic<br />

no. 621571240<strong>2.</strong><br />

REFEREnCES<br />

1. Shao Y. et al.: Flavour and Fragrance Journal 18, 5<br />

(2003).<br />

<strong>2.</strong> López P., et al.: Analytica Chimica Acta 559, 97 (2006).<br />

3. Holadová K., Prokůpková G., Hajšlová J., et al.: Analytica<br />

Chimica Acta 582, 24 (2007).

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