• Food Science and Biotechnology
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• 제16권1호
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• pp.37-42
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• 2007

The biotransformation of monoterpenic agro-industrial wastes (turpentine oil and essential orange oil) was studied. More than 40 fungal strains were isolated from Brazilian tropical fruits and eucalyptus trees and screened for biotransformation of the waste substrates. Solid phase microextraction was used to monitor the presence of volatile compounds in the headspaces of sporulated surface cultures. The selected strains were submitted to submerged liquid culture. The biotransformation of R-(+)-limonene and ${\alpha},\;{\beta}-$ pinenes from the oils resulted in ${\alpha}-terpineol$ and perillyl alcohol, and verbenol and verbenone, respectively, as the main products. The selected strains were also placed in contact with ${\alpha}-$ and ${\beta}-$ pinenes standards. It was confirmed that verbenol, verbenone, and ${\alpha}-terpineol$ were biotransformation products from the terpenes. A concentration of 90 mg/L of verbenone was achieved by Penicillium sp. 2360 after 3 days of biotransformation.

• 분석과학
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• 제20권2호
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• pp.115-123
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• 2007

헤테로싸이클릭 아민류(heterocyclic amines, HAs)는 소고기, 돼지고기, 닭고기 그리고 생선과 같은 근육질의 육류를 조리 할 때 생겨나는 돌연변이원성/발암성 화학물질로 잘 알려져 있다. 식품으로부터 HAs의 분석에 있어 가장 큰 어려움은 HAs가 식품 중에 극히 미량(수 ng/g)으로 존재한다는 것과 많은 방해물질이 존재한다는 것이다. 식품으로부터 HAs를 추출하고 정제하기 위해 고체-상 추출(solid-phase extraction, SPE)이 많이 사용되고 있다. HAs 분석을 위해 여러 단계의 SPE 과정을 수행하였다. HAs의 회수율은 표준물질이 녹여져 있는 메탄올 수용액과 조리되지 않은 돼지고기에 표준용액을 스파이크하여 서로를 비교하여 얻었다. 회수율은 25.0 ng/g에서 25.3~93.0%의 값을 얻을 수 있었다. 확립된 감도 좋고 재현성있는 시료전처리방법을 통해서 ${\mu}$-LC/ESI-MS에 주입함으로써 조리된 육류로부터 HAs를 분석하는데 응용될 수 있을 것이다. 다른 방법으로는 freezing filtration 방법으로써 보다 좋은 추출 효율과 재현성을 나타내었다.

• 대한화학회지
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• 제45권6호
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• pp.524-531
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• 2001

Microcystin-LR, -YR 및 -RR과 같은 독성 microcystin의 분석에 있어서 정확성을 높이기 우해 고상 추출을 통한 micro-HPLC/IS/MS를 사용하였다. 이러한 microcystin-LR, -YR, -RR를 확인하는데 HPLC/UV로는 238nm에서의 흡광도를 측정하였고, 질량스펙트럼에서는 1 35m/z 및 $[M+H]^+$m/z의 특성 피이크만을 검출하여 왔다. 본 연구에서는 이중 전하에 해당하는 새로운 선들이 LR에서는 507m/z, PR에서는m/z, YR에서는 532m/z에서 추가로 검출되었다. 이 방법을 사용하여 대청호에서 독성 microcystin의 존재성을 조사하였다.

• 한국지하수토양환경학회지:지하수토양환경
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• 제15권1호
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• pp.9-18
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• 2010

In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

• 한국수산과학회지
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• 제42권3호
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• pp.224-231
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• 2009

Volatile components in Olive Flounder fed diets containing 0, 2,5, 5.0, and 7.5% yuza (Citrus junas Sieb ex Tanaka) for 4 months were investigated. Samples were extracted by solid-phase micro extraction and analyzed by gas chromatography/mass spectrometry. Among 89 compounds detected, 82 were positively identified. Volatile compounds of Olive Flounder fed the unsupplemented diet comprised 12 acids, 10 alcohols, eight aldehydes, five aromatic compounds, nine esters, 12 hydrocarbons, four ketones, two monoterpenes, and one miscellaneous compound. Compounds identified in Olive Flounder fed the yuza-supplemented diets consisted of 10 esters, 11 monoterpenes, 13 sesquiterpenes, and two miscellaneous compounds, with the other compounds being the same as in the control. The most abundant class of compounds in flounders fed the yuza-supplemented diet was the monoterpenes, which included limonene, $\beta$-terpinene, $\beta$-trans-ocimene, and $\alpha$-terpinolene. Of the 13 sesquiterpenes identified in flounder fed the yuza-supplemented diet, bicyclogermacrene was the major volatile compound followed by allo-aromadendrene, trans-caryophyllene, and $\delta$-cadinene. Bicyclogermacrene and germacrene D content increased significantly as the yuza supplementation increased.

• 분석과학
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• 제25권5호
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• pp.292-299
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• 2012

GC/MS (gas chromatography/mass spectrometry)는 훌륭한 분리능과 재현성으로 인해 널리 활용되고 있으며, 정립된 데이터베이스의 활용을 통한 성분 분석에서 활용도가 높다. 또한 HS-SPME (headspacesolid phase micro extraction)법은 용매로 추출을 하지 않은 휘발성 물질의 추출을 하는데 널리 사용되었다. 이 두 방법의 연계는 다양한 시료에서 발생하는 휘발성 성분의 분석에 널리 활용되었다. 위 특징을 이용하여 살아있는 Camponotus japonicus가 분비하는 미량의 페로몬 구성 성분의 분석 방법을 확립하였다. n-Decane, n-undecane, n-tridecane 등의 물질이 미량 페로몬에서 검출되었으며, 이 탄화수소들을 분석하는데 적합한 SPME fiber, 추출 온도, 추출 시간을 최적화하였다. 살아있는 시료를 분석할 수 있기 때문에 특정 현상이 발생하는 그 순간을 분석하는 장점이 있는 한편, 살아있는 시료를 분석하기 때문에 추출 시간 등이 제한된다는 한계점이 있었으나 살아있는 HS-SPME GC/MS 분석방법이 정립된다면 살아있는 시료를 죽일 필요 없다는 점에서 친환경적인 연구의 발전에 해결책이 될 수 있을 것으로 전망한다.

• 한국식품영양학회지
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• 제31권6호
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• pp.890-896
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• 2018

The aim of this study was to determine volatile flavor compounds in Shingo pear juice. Volatile flavor compounds were analyzed using solid-phase micro-extraction (SPME) - gas chromatography-mass spectrometry (GC-MS). The effect of inorganic salts solution on the extraction ability of the SPME fiber was treated by adding saturated $CaCl_2$ solution at the ratio of 1:20 (v/v) after 0, 60, 120 min of preparing pear juice, respectively. As a result, a total of 22 volatile compounds were identified in Shingo pear juice. Ethyl acetate was found to be the most abundant volatile compound ($13.36{\sim}19.61{\mu}g/kg$), followed in order by hexanal, ethyl hexanoate, ethyl 3-(methylthio)-2-propenoate, ethyl octanoate and 2-hexenal. Total contents of volatile flavor compounds were $31.07{\mu}g/kg$ (control), $40.93{\mu}g/kg$ (0 min), $27.62{\mu}g/kg$ (60 min) and $26.32{\mu}g/kg$ (120 min). This result indicated that the addition of saline solutions could inhibit the enzymatic reaction of volatile flavor compounds effectively when treated as soon as juice preparation.

• Toxicological Research
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• 제31권3호
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• pp.273-278
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• 2015

The aim of this study was to develop an efficient quantitative method for the determination of acetaldehyde (AA) and formaldehyde (FA) contents in solid and liquid food matrices. The determination of those compounds was validated and performed using gas chromatography-mass spectrometry combined by solid phase micro-extraction after derivatization with O-(2,3,4,5,6-pentafluoro-benzyl)-hydroxylamine hydrochloride. Validation was carried out in terms of limit of detection, limit of quantitation, linearity, precision, and recovery. Then their contents were analyzed in various food samples including 15 fruits, 22 milk products, 31 alcohol-free beverages, and 13 alcoholic beverages. The highest contents of AA and FA were determined in a white wine (40,607.02 ng/g) and an instant coffee (1,522.46 ng/g), respectively.

• Bulletin of the Korean Chemical Society
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• 제28권3호
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• 한국연초학회지
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• 제32권2호
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• pp.77-87
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• 2010

Traditional simultaneous distillation extraction(SDE) and solid-phase micro extraction(SPME) methods using GC/MS were compared for their effectiveness in the extraction of volatile flavor compounds from different tobacco leaves types(flue-cured, burley, oriental). The major volatile flavor compounds of flue-cured and burley tobacco were similar such as neophytadiene, solanone, megastigmatrienone isomers, ${\beta}$-damascenone and ${\beta}$-ionone. On the other hand, volatile flavor compounds such as norambreinolide, sclareolide were specifically identified in oriental tobacco. Each method was used to evaluate the responses of some analytes from real samples and standards in order to provide sensitivity comparisons between two techniques. Among three types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate) and PDMS/DVB (Polydimethylsiloxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency, PDMS/DVB fiber was selected for the extractions of the volatile flavor compounds due to its effectiveness. The qualitative analysis showed that the total amount of volatile flavor compounds in SDE method(130 species) was much more than that in SPME method(85 species). SPME method was more efficient for all the highly volatile compounds than SDE method, but on the other hand, low-volatile compounds such as fatty acids or high-molecular hydrocabons were detected in SDE method. SPME method based on a short-time sampling can be adjusted to favor a selected group compounds in tobacco. Furthermore this results could be used to estimate the aroma characteristics of cigarette blending by using a different type of tobacco with more effectiveness and convenience.