• Food Science and Biotechnology
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• v.18 no.1
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• pp.66-72
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• 2009

An aqueous ribose-cysteine model system (initial pH 5.6) was conventionally heated to the same browning at varying temperatures ($120-180^{\circ}C$), supercritical carbon dioxide (SC-$CO_2$, 20 MPa) was also applied on the same matrices for same periods at each temperature and about 20% reduction of the absorbance at 420 nm was observed as compared with sole thermal treatment. The headspace volatiles from Maillard reaction mixtures were analyzed by solid-phase microextraction (SPME) in combination with gas chromatography and mass spectrometry (GC-MS), and predominated with sulfur containing compounds, such as thienothiophenes, polysulfur alicyclics, thiols, and disulfides. Reaction temperature exhibited complex effects on volatiles formation and those effects became further complicated by the SC-$CO_2$ treatment. The formation of noncarbonyl polysulfur heterocyclic compounds and thienothiophenes was generally favored at high temperatures. Most volatiles were inhibited in SC-$CO_2$ as compared with thermal treatment alone, however, the well-known meaty aromatic compounds, such as thiols and disulfides, were obviously enhanced.

• Bulletin of the Korean Chemical Society
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• v.32 no.10
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• pp.3603-3609
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• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.5
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• pp.783-789
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• 2000

This study was focused on the optimal extracting conditions of dimethyl-$\beta$-propiothetin as bioactive substance from green seaweed. Identification and quantification of dimethyl-$\beta$-propiothetin were measured by headspace gas chromatography after conversion to dimethyl sulfide by treatment with saturated NaOH solution. Dimethyl-$\beta$-propiothetin was extracted through various processes (solvent extraction, ultrasonication, boiling and autoclaving) from Ulva pertusa. The content of dimethyl-$\beta$-propiothetin extracted by autoclaving treatment showed higher than that of various extraction methods. Dimethyl-$\beta$-propiothetin content in extract of Ulva pertusa was 325,800 ng/g after autoclaving 121$^{\circ}C$ for 45 min. Dimethyl-$\beta$-propiothetin in exract of Ulva pertusa was comparative stable under low temperature. The retentions of dimethyl-$\beta$-propiothetin content in extract of Ulva pertusa were 76.6~99.8% by incubation at 10~6$0^{\circ}C$ for 2 hours. Chemical decomposition of dimethyl-$\beta$-propiothetin was observed under laboratory conditions at pH values higher than 9.5.

• Analytical Science and Technology
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• v.24 no.6
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• pp.421-428
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• 2011

In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

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

• Culinary science and hospitality research
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• v.19 no.3
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• pp.105-115
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• 2013

Maillard reaction flavors had been tried by using krill hydrolysate and precursors in order to develop Teriyaki sauce with the reaction flavors. Also, the study for applying krill to Teriyaki sauce had been tried by using krill instead of eel bones. To make boiled-type and grilled-type reaction flavors, krill hydrolysate was used with other precursors such as serine, glucose and glucosamine. In the dynamic analysis of headspace volatile compounds, 20 mL reaction flavor was analyzed by the combined system of purge & trap, automatic desorber, gas chromatography and mass selective detector. Three kinds of Teriyaki sauce were developed with reaction flavor, krill and eel bones, and their products were evaluated by 10 items of cooked vegetables, cooked potatoes, boiled shrimp, grilled shrimp, fishy smell, pungent aroma, burned smell, sweety aroma, chemical smell, mud smell and preference. In the results of headspace analysis, 35 and 33 volatile compounds were identified from grilled-type and boiled-type reaction flavors. Grilled-type had sulfur-containing, aliphatic compounds, alcohols, ketones, pyrazines, and other aromatic compounds, and grilled-type had aldehydes, furans, other nitrogen-containing compounds. In the sensory evaluation of Teriyaki sauce, the items of roasted shrimp and sweety aroma showed significant differences for grilled-type application to Teriyaki sauce. The above results show the possible application of grilled-type reaction flavor to Teriyaki sauce.

• Journal of Life Science
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• v.28 no.12
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• pp.1523-1528
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• 2018

This study investigated the chemical composition of four Korean cultivated Chrysanthemum indicum L. (Gamguk 1 ho, Gamguk 2 ho, Gamguk 3 ho, and Wonhyang) which are used in the food and fragrance industries to identify their volatile flavor compounds. These compounds were analyzed using headspace GC-MS from plant samples cultivated in the same region of Korea (Sancheong-gun, Gyeongsangnam-do). A total of 23 compounds were identified, eight of which were common across the four cultivars. The major flavor components in the three Gamguk plants were identified as 3-carene, camphene, ${\beta}$-phellandrene, eucalyptol and (+)-camphor. Eleven compounds, including (+)-camphor at 31.40%, were identified in Gamguk 1 ho. Gamguk 2 ho was found to contain 12 flavor compounds, predominant of which was camphene at 25.60%. Thirteen compounds including (+)-camphor (26.88%) were identified in Gamguk 3 ho, while 17 were detected in the Wonhyang cultivar, including trans-piperitol (47.33%), sabinene, and ${\gamma}$-terpinyl acetate. These results indicate differences in the type and ratio of functional volatile flavor ingredients in Chrysanthemum indicum L. cultivars which is highly valuable as material for fragrance product development.

• Applied Biological Chemistry
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• v.29 no.2
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• pp.190-197
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• 1986

In order to develop a simple and effective method for determining the rate of the Maillard reaction in non-fat dry milk, the carbon dioxide content of the headspace as an indicator were used and the amount of correlation between $CO_2$ content and brown color development were determined by the gas chromatograph. There is a high correlation between brown color and $CO_2$ content. The use of gas chromatography to analyze the $CO_2$ in the headspace of samples is a quick, simple and effective method of monitoring the Maillard reaction. Volatile concentration increases with storage time and varies inversely with oxygen content. Lysine is more effective than glucose in catalyzing the Maillard reaction. Product samples can be stored at $55^{\circ}C$ and $68^{\circ}C$ to accelerate the rate of the Maillard reaction and shorten testing period, but product stored at $75^{\circ}C$ is degraded too rapidly to be of any real use.

• Food Engineering Progress
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• v.14 no.3
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• pp.249-255
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• 2010

Ten commercial activated carbons (ACs) prepared from four different sources (bamboo, wood, peat, and coal) were evaluated for their adsorptive efficiency of six volatile compounds (isoamyl alcohol, hexanal, furfural, ethyl lactate, ethyl octanoate, 2-phenyl ethanol) which were dissolved in a 30% alcoholic model solution. These six volatile compounds are frequently found in alcoholic beverages and possibly contribute to physiological hangover due to their high concentrations. They are also generally regarded as off-flavor compounds at certain levels in alcoholic beverages such as whisky and vodka. Two hundred mL of 30% alcoholic solutions containing these six volatile compounds were treated with 0.2 g of ACs while stirring for 16 hr; the treated solutions were then measured for their adsorptive efficiencies (or removal efficiencies) by gas chromatographic analysis using two different sampling methods (direct liquid injection and headspace-solid phase microextraction). The adsorptive efficiencies of the ACs varied depending on the identity of the volatile compounds and the source material used for making the ACs. Ethyl octanoate, 2-phenyl ethanol, and hexanal were removed at high efficiencies (34-100%), whereas isoamyl alcohol, ethyl lactate, and furfural were removed at low efficiencies (5-13%). AC prepared from bamboo showed a high removal efficiency for isoamyl alcohol, aldehydes (hexanal and furfural), and 2-phenyl ethanol; these major fusel oils have been implicated as congeners responsible for alcohol hangover.

• Analytical Science and Technology
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• v.28 no.6
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• pp.436-445
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• 2015

Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.