Characterization of volatile components in dry chrysanthemum flowers using headspace-liquid-phase microextraction-gas chromatography.
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 microg/g), camphene (112.7 microg/g), eucapyptol (52.1 microg/g), camphor (29.4 microg/g), borneol (4.2 microg g), bornyl acetate (67.3 microg/g), caryophyllene (0.7 microg/g), and caryophyllene oxide (20.0 microg/g). The relative standard error and detection limit of this method is 5-9% and 0.4 microg/g, respectively.
Wang
Guoqing
G
Department of Applied Chemistry, Zhengzhou University of Light Industry, Zhengzhou, Henan, 450002, China. gqwang@ustc.edu
Dong
Chunhong
C
Sun
Yu-an
YA
Xie
Kui
K
Zheng
Haiyu
H
D005591:Chemical Fractionation / Q000379:methods; D031202:Chrysanthemum / Q000737:chemistry*; D004365:Drugs, Chinese Herbal / Q000737:chemistry* / Q000302:isolation & purification; D035264:Flowers / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009822:Oils, Volatile / Q000737:chemistry* / Q000302:isolation & purification; D012965:Sodium Chloride; D012995:Solubility; D013696:Temperature; D013997:Time Factors
D004365:Drugs, Chinese Herbal; D009822:Oils, Volatile; D012965:Sodium Chloride