Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
46, Number 2, February 2008, pp. 127-132
Characterization of Volatile Components in Dry
Chrysanthemum Flowers Using Headspace–Liquid- Phase Microextraction–Gas
Chromatography
Guoqing Wang[1], Chunhong Dong[2], Yu-an Sun[1], Kui
Xie[3], and Haiyu Zheng[1]
[1]Department of Applied Chemistry, Zhengzhou University of Light
Industry, Zhengzhou, Henan, 450002;
[2]Department of Science
and Technology, Jiaozuo University, Jiaozuo, Henan, 454003; and
[3]Henan Center for Disease Control and Prevention, Zhengzhou,
Henan, 450003, China
A headspace–liquid-phase microextraction
(HS–LPME)–GC (gas chromatography) method for the
characterization of volatile components in dry chrysanthemum
flowers has been developed. In the proposed method, two extraction
solvents, n-hexadecane and benzyl alcohol, are used for preconcentrating
volatiles in the sample. A droplet of the extraction solvent
is squeezed from the GC syringe and inserted in the headspace
of the sample bottle with the dry flower, immersed in deionized
water, and warmed in a water bath. The optimum HS–LPME
parameters in terms of extraction solvent type, droplet magnitude,
equilibrium (water bath) temperature, equilibrium time, extraction
time, and ionic strength are achieved using GC–FID (flame
ionization detection) by varying several levels of the factors
that affect the HS–LPME procedure. After extraction under
the optimized conditions, the extraction droplet is retracted
into the syringe and injected for GC–MS (mass spectrometry)
analysis. Thirty-three volatile components are extracted and
identified using this HS–LPME–GC–MS method,
with the aid of chemometric methods. It is shown that the volatiles
in dry chrysanthemum flowers are mainly unsaturated organic compounds,
such as monoterpenes, sesquiterpenes and their oxygenous derivatives,
triterpenoids, and aliphatic compounds. Several representative
components, in order of precedence of the retention time, are
pinene (106.3 µg/g), camphene (112.7 µg/g), eucapyptol
(52.1 µg/g), camphor (29.4 µg/g), borneol (4.2 µg
g), bornyl acetate (67.3 µg/g), caryophyllene (0.7 µg/g),
and caryophyllene oxide (20.0 µg/g). The relative standard
error and detection limit of this method is 5~9% and 0.4 µg/g,
respectively.
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