• 한국식품과학회지
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• 제38권6호
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• pp.738-741
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• 2006

본 실험에서는 시판중인 우유 4종을 대상으로 static headspace, purge and trap 및 SPME의 세 가지 향기성분 추출방법을 이용하여, GC/MS로 각각의 향기성분을 분석하였다. Purge and trap법을 이용한 분석법으로 가장 많은 종류의 성분을 분석할 수 있었으며, 향기성분의 추출효율이 가장 좋았다. SPME법은 간단한 장비로 신속하게 향기성분을 포집할 수 있는 장점이 있으며, 추출 효율 또한 뛰어나 효율적인 향기성분 분석방법으로 이용이 가능하였다. 4종의 시판우유 중에서 검출된 향기성분은 대체적으로 큰 차이를 나타내지 않았으나, 다소의 양적차이를 나타내었다. 검출 된 성분은 주로 acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone 등의 케톤류, pentanal, 2-methylbutanal, hexanal, benzaldehyde 등의 알데하이류 및 dimethyl sulfide 등의 황화합물류로써, 우유의 주요 이취성분들이었다.

• 분석과학
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• 제18권3호
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• pp.224-231
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• 2005

잔류농약 분석에 전통적으로 사용되는 액체-액체 추출법과 액체-고체 추출법의 여러 가지 단점을 극복하고 기존의 낮은 정밀도와 저조한 추출효과를 보완하기위해 자동화된 장치를 이용한 액체상 극미량 추출법(Liquid Phase Microextraction : LPME)을 사용하였으며 이에 대한 최적화 조건을 설정하였다. 대상농약은 demeton-S-methyl, diazinon, parathion, fenitrothion, EPN등 5종이었으며 채소 시료 중에서 추출하여 HP 6890 GC/NPD를 사용하여 분석하였다. 자동화된 LPME를 이용한 최적의 추출조건은 pH 3, 염의 농도 $100{\mu}g/mL$이었으며 검량선을 작성하였을 때 $0.2{\sim}10{\mu}g/g$ 범위에서 $R^2=0.9921$ 이상 직선상의 상관관계를 나타내었고 $5{\mu}g/g$ 농도에서 demeton-S-methyl은 7.7%, diazinon은 9.8%, parathion은 7.8%, fenitrothion는 9.7%, EPN은 8.2%의 상대표준편차를 나타내었고 정확도는 demeton-S-methyl는 12.7%, diazinon는 7.8%, parathion는 10.4%, fenitrothion는 -6.7%, EPN은 -0.7%로 좋은 값을 나타내었다.

• Bulletin of the Korean Chemical Society
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• 제32권11호
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• pp.3923-3927
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• 2011

A noble method for pre-concentration and speciation of ultra trace As (III) and As (V) in urine and whole blood samples based on dispersive liquid-liquid microextraction (DLLME) has been developed. In this method, As (III) was complexed with ammonium pyrrolidine dithiocarbamate at pH = 4 and Then, As (III) was extracted into the ionic liquid (IL). Finally, As (III) was back-extracted from the IL with hydrochloric acid (HCl) and its concentration was determined by flow injection coupled with hydride generation atomic absorption spectrometry (FI-HGAAS). Total amount of arsenic was determined by reducing As (V) to As (III) with potassium iodide (KI) and ascorbic acid in HCl solution and then, As (V) was calculated by the subtracting the total arsenic and As (III) content. Under the optimum conditions, for 5-15 mL of blood and urine samples, the detection limit ($3{\sigma}$) and linear range were achieved 5 ng $L^{-1}$ and 0.02-10 ${\mu}g\;L^{-1}$, respectively. The method was applied successfully to the speciation and determination of As (III) and As (V) in biological samples of multiple sclerosis patients with suitable precision results (RSD < 5%). Validation of the methodology was performed by the standard reference material (CRM).

• Food Science and Biotechnology
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• 제18권4호
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• pp.895-899
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• 2009

A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.

• Food Science and Biotechnology
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• 제14권2호
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• pp.238-241
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• 2005

Aroma-active compounds were evaluated from salt-fermented anchovy sauce by solid phase microextraction-gas chromatography-olfactometry (SPME-GC-O) based on sample dilution analysis (SDA). SPME extract from carboxen/polydimethylsiloxane (CAR/PDMS) fiber was the most similar to the original odor of salt-fermented anchovy sauce used for this experiment, followed by divinylbenzene/CAR/PDMS (DVB/CAR/PDMS) fiber. Because salt-fermented anchovy sauce contains 23% NaCl, NaCl concentration of diluent was considered when salt-fermented anchovy sauce was serially diluted. Linear relationship between GC response and sample concentration was observed when diluted with 23% NaCl solution, whereas not observed when diluted with deodorized distilled water. Eleven and 16 aroma-active compounds were detected by SPME-GC-O based on SDA using CAR/PDMS and DVB/CAR/PDMS fibers, respectively. Butanoic acid and 3-methyl butanoic acid showed the highest ${\log}_2SD$ factors for CAR/PDMS and DVB/CAR/PDMS fibers. Dimethyl trisulfide, methional, trimethyl amine, 1-penten-3-ol, and acetic acid were also detected as potent aroma-active compounds.

• 한국식품위생안전성학회지
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• 제14권1호
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• pp.76-83
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• 1999

Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

• 분석과학
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• 제33권2호
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• pp.76-85
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• 2020

A stainless-steel needle (Hamilton 90022, 22 gauge, 718-㎛ o.d., 413-㎛ i.d., 51-mm length, bevel tip) with an electrochemically coated polyaniline layer having a microbore tunnel was newly prepared as a device for headspace in-needle microextraction. For designing the needle, the polyaniline layer length was optimized, and to evaluate the extraction efficiency for polycyclic aromatic hydrocarbons, numerous cyclic voltammetry scans were conducted. In addition, the optimization of the analytical conditions (including the adsorption and desorption parameters) and the validation of the analytical method were conducted. The optimized adsorption and desorption conditions were 40 ℃ for 30 min and 230 ℃ for 60 s, respectively. Finally, in this study, a polyaniline layer was electrochemically deposited on the in-needle surface, and it exhibited good thermal stability. The needle with the polyaniline layer was repeatedly used more than 200 times during this study. This method has some advantages in terms of the extraction time, extraction efficiency, and analysis cost.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.211-217
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• 2014

A new needle-based device for headspace wire coated in-needle microextraction (HS-WC-INME) was fabricated using a nichrome wire coated with poly(ethylene glycol) (PEG) and poly(dimethylsiloxane) (PDMS) mixture. The proposed needle device was applied for the determination of volatile compounds in lavender and lavandin essential oils by gas chromatography. Fundamental parameters such as needle design, conditions of extraction and desorption were optimized along with the validation of the extraction and desorption efficiency. The optimal conditions were 30 min extraction at $50^{\circ}C$ and 2 min desorption at $240^{\circ}C$. The calibration curves showed good linearity with the suitable values of the coefficients of determination ($r^2$) greater than 0.99. The limits of detection for linalyl acetate, ${\beta}$-caryophyllene, linalool and (+)-limonene were 7.15, 9.04, 10.79 and 22.26 ng, respectively. Analytical recoveries were acceptable in the test samples, varying from 86.7% to 108.0%. The values of relative standard deviations for run to run showed range less than 0.9% while 3.9% through 7.2% for needle to needle. The proposed PEG-PDMS coating could be more suitable than PDMS coating to extract particular polar groups such as alcohols.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.231-236
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• 2006

A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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• pp.49-52
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• 2009

Single-drop microextraction (SDME) is an extraction methodology where the drop plays an essential role as extracts. It was evaluated for the GC-MS determination of nerve agents, one class of the chemical warfare agents (CWAs). Since these nerve agents are highly toxic, it is important to detect the nerve agents in the environmental samples. Several affecting factors including extraction solvents, stirring rate, extraction time, and amounts of salt were optimized. The limit of detections (LODs) were 0.1 - 10 ng/mL and the relative standard deviations (RSDs%, n=5) were in the range of 6.3% to 9.0% for four nerve agents. Without pretreatment of the environmental samples, 5-103 fold enrichments and 48-100% recovery were accomplished. These results demonstrated the feasibility of this method for on-site and off-site analysis of water sample collected from suspicious CWAs site.