• Korean Journal of Food Science and Technology
• /
• v.38 no.6
• /
• pp.738-741
• /
• 2006

Volatile flavor compounds in commercial sterilized milk were analyzed and identified by static headspace, purge-and-trap, and solid-phase microextraction (SPME) methods. About 20 volatile compounds were identified by GC/MS, and aldehydes and ketones were the most distinctive and abundant compounds. Static headspace analysis allowed the identification of only the most abundant compounds, such as acetone. Five ketones (acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone), four aldehydes (2-methylbutanal, pentanal, hexanal, benzaldehyde) and dimethyl sulfide, all of which were responsible for off-flavor in milk, were found by the purge-and-trap and SPME methods. The two methods differed little in their release of these compounds, but they yielded different amounts in the extraction.

• Bulletin of the Korean Chemical Society
• /
• v.25 no.2
• /
• pp.271-279
• /
• 2004

The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.

• Analytical Science and Technology
• /
• v.14 no.5
• /
• pp.392-399
• /
• 2001

The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

• Analytical Science and Technology
• /
• v.30 no.2
• /
• pp.68-74
• /
• 2017

The volatile components in 'Fuji' apple were effectively determined by a headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 48 volatile components were identified and tentatively characterized based on National Institute of Standards and Technology (NIST) MS spectra library and the Kovats GC retention index I (RI). The harvested Fuji apples were divided into two groups: 1-methylcyclopropene (1-MCP) treated and non-treated (control) samples for finding important indicators between two groups. The major volatile components of both apples were 2-methylbutyl acetate, hexyl acetate, butyl 2-methylbutanoate, hexyl butanoate, hexyl 2-methylbutanoate, hexyl hexanoate and farnesene. No significant differences of these major compounds between 1-MCP treated and non-treated apples were observed during 1 month storage. Interestingly, the amount of off-flavors, including 1-butanol and butyl butanoate, in 1-MCP treated apples decreased over 5 months, and then increased after 7 months. However, non-treated apples did not show significant changes for off-flavors during 7 month storage (p<0.05). The non-treated apples also contained the higher levels of two off-flavors than 1-MCP treated apples. These two compounds, 1-butanol and butyl butanoate, can be used as quality indicators for the quality evaluation of Fuji apple.

• Mass Spectrometry Letters
• /
• v.8 no.1
• /
• pp.18-22
• /
• 2017

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

• Journal of the Korean Society for Marine Environment & Energy
• /
• v.17 no.1
• /
• pp.27-35
• /
• 2014

The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

• Korean Journal of Food Science and Technology
• /
• v.32 no.3
• /
• pp.507-512
• /
• 2000

The headspace flavors of roasted tea, prepared with steamed and nonsteamed polygonatum roots, were absorbed in solid-phase microextraction(SPME) fiber coated with $65\;{\mu}m$ of carbowax/divinylbenzene(CW/DVB) and analysed by GC-MS. The absorption conditions of SPME fiber for equilibrated headspace were selected as $60^{\circ}C$ and 30 min. In a comparison for both samples roasted at $130^{\circ}C$ for 15 min, gas chromatograms showed a similar pattern in overall profiles between steamed and nonsteamed samples before roasting, but some differences were observed in peak characteristics. From 40 separated peaks, 25 compounds were identified with both GC-MS and retention time comparison. The pyrazines including 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, 2,5-dimethyl-4-hydroxy-3(2H)-furanone, 2-acetyl-1-pyrroline, etc. were higher in their contents in nonsteamed-roasted sample than steamed-roasted one. In particular, steamed-roasted polygonatum showed higher contents of acetic acid(8.17%) and hexanoic acid(5.43%) than the corresponding compounds of nonsteamed-roasted one, 2.40% and 2.00%.

• Analytical Science and Technology
• /
• v.20 no.3
• /
• pp.237-245
• /
• 2007

The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

• Applied Biological Chemistry
• /
• v.51 no.3
• /
• pp.233-237
• /
• 2008

The essential oil was obtained from the aerial part of Rhododendon mucronulatum Turcz. var. ciliatum Nakai by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the oil were analyzed by gas chromatography-mass spectrometry (GC-MS). Nineteen constituents were identified from the essential oil: 15 carbohydrates, 3 alcohols, and 1 acetates. Major constituents were 2-${\beta}$-pinene (16.1%), camphene (11.9%), ${\delta}$-3-carene (11.4%), d,l-limonene (9.5%), and ${\gamma}$-terpinene (9.5%). By SPME extraction, seventeen constituents were identified: 13 hydrocarbons, 1 alcohol, 1 nitrogen-containing compound, 1 acetate, and 1 amine. Major constituents of the SPME-extracted sample were cam phene (19.6%), 2-${\beta}$-pinene (18.0%), ${\delta}$-3-carene (17.4%), trimethyl hydrazine (9.7%), ${\gamma}$-terpinene (8.5%), and d,l-limonene (5.5%). By HS extraction, thirteen constituents were identified: 11 hydrocarbons, 1 alcohol, and 1 nitrogen-containing compound. Major constituents of the HS-extracted sample were camphene (25.8%), ${\delta}$-3-carene (24.8%), 2-${\beta}$-pinene (20.2%), d,l-limonene (5.4%), tricyclene (5.1%) and trimethyl hydrazine (4.6%). The fragrance of the essential oil was coniferous, balsamic, and woody, and the $IC_{50}$ value of the essential oil was 0.030 ${\mu}g/mg$ in MTT assay using UaCaT keratinocyte cell line.

• The Korean Journal of Food And Nutrition
• /
• v.19 no.2
• /
• pp.161-168
• /
• 2006

The efficiency of six different extraction methods for the analysis of aroma components from pine needle(P. densiflora) was compared by gas chromatography-mass selective detector(GC-MSD). The six methods were dynamic headspace(DHS), reduced pressure headspace(RPHS), solid-phase microextraction(SPME), simultaneous distillation-extraction(SDE), supercritical fluid extraction(SFE) and pyrolysis distillation extraction(PDE). A total of 65 compounds were identified by using the six different extraction methods. These compounds are classified into six categories in terms of chemical functionality: 25 hydrocarbons, 16 alcohols, 9 carbonyls, 6 esters, 7 acids, and 2 ethers. The aroma compounds having low boiling point were more abundant in DHS, RPHS, and SPME extracts. On the other hand, the aroma compounds having high boiling point were more abundants in SDE, SFE and PDE extracts. The acid compounds were extracted by heat-based extraction methods such as SDE, SFE, PDE, but not by DHS, RPHS and SPME, which used neither solvent nor heat. The oxygenated terpens, hexanal, hexanol, and hexadienal were more abundant in DHS and RPHS extracts, compared with the other methods.