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

• 분석과학
• /
• 제20권5호
• /
• pp.370-382
• /
• 2007

본 연구에서는 GC/FID를 이용한 SPME법을 적용하여 액상에서 대표적 디젤첨가제인 EGBE, DGBE, DBM, TGME의 미량 분석 가능성을 조사하였다. 또한, 요인배치설계법을 적용하여 EGBE, DGBE, DBM, TGME 미량분석의 최적조건을 도출하였다. 실험은 통계분석결과 뿐만 아니라 요인 수의 최적화에 따른 중심합성설계에 의한 완전요인 설계법을 사용하였으며, 반응표면분석은 추출 효율이 주 영향인염 농도, 흡착 온도, 흡착 시간과 sonication 시간에 따른 2차 다항식에 의해 설명될 수 있음을 보여주었다. 본 연구에서의 결과는 요인배치설계법을 사용하여 액상 시료에서 EGBE, DGBE, DBM, TGME의 정량분석을 개선하는 새로운 자료분석법을 보여주었다.

• 한국축산식품학회지
• /
• 제33권5호
• /
• pp.646-654
• /
• 2013

본 연구에서는 발효유의 휘발성 향기성분을 HS-SPME/GC-FID를 이용하여 정량분석의 가능성을 검토하고, 정량 분석의 재현성 및 정확성을 확인하여 발효유의 휘발성 향기성분 연구에 접목시키고자 실험을 실시하였다. HS-SPME를 이용하여 발효유의 acetaldehyde, acetone, diacetyl 그리고 acetoin 등의 향기성분 추출 시 $35^{\circ}C$에서 가장 효과적으로 추출할 수 있었다. 그리고 발효유의 주요 휘발성 향기성분의 표준물질을 농도별로 제조하여 standard curve를 작성하여 상관관계식을 얻을 수 있었으며, $r^2$값은 모든 표준시료에서 0.9979 이상으로 뛰어난 상관관계를 나타냈다. 곡류(백미, 현미, 발아현미, 발아현미당화)를 첨가한 발효유를 제조하여 저장기간 중 휘발성 향기성분의 함량변화를 비교분석하였다. Acetaldehyde의 경우 대조구 및 백미첨가 발효유는 저장기간 중 acetaldehyde의 함량이 약 1.4배 증가하였다. 현미와 발아현미, 그리고 발아현미 당화액을 첨가한 발효유의 경우 저장 0일차 acetaldehyde의 함량이 11.78, 12.39, 12.15 ppm으로 대조구의 0일차 함량(10.83 ppm)보다 높은 함량을 나타냈지만, 저장 15일차에는 acetaldehyde 함량이 각각 11.96, 13.04, 12.10 ppm으로 대조구의 15일차 함량(15.67 ppm)보다 약 1.3배 낮은 함량을 나타냈다. Acetone은 매우 미량으로 분석되었고, 저장기간 중 생성 또는 휘발되어 유의적인 차이는 없었다(p<0.05). 대조구 및 백미첨가발효유의 diacetyl 함량은 저장기간 중 약 2배 증가하였고, 현미와 발아현미, 그리고 발아현미 당화액 첨가 발효유의 경우 저장 0일차 함량이 각각 0.74, 0.81, 0.84 ppm으로 대조구 및 백미첨가발효유의 함량(0.35, 0.48 ppm)보다 높게 분석되었다. Acetoin 함량은 곡류를 첨가한 발효유에서 대조구보다 전체적으로 높은 함량을 나타냈고, 대조구 및 백미첨가발효유의 경우 저장기간 중 유의적인 변화를 보이지 않았으며(p<0.05), 현미와 발아현미 그리고 발아현미 당화액 첨가 발효유는 저장기간 중 감소하는 경향을 나타냈다. HS-SPME/GC를 이용하여 곡류를 첨가한 발효유의 저장 기간 중 휘발성 향기성분의 변화를 정량 분석한 결과 재현성이 뛰어났으며, 개별 향기성분의 분석도 가능하였다. 따라서 발효유의 휘발성 향기성분을 고가의 장비를 사용하지 않고 간편하고 효율적으로 추출할 수 있는 HS-SPME/GC를 이용하여 정량분석이 가능할 것으로 판단되며, 발효유의 휘발성 향기성분 분석 및 제조 및 품질특성에 관한 기초 연구 시 경제적이고 효율적으로 이용가능할 것으로 판단된다.

• 한국지하수토양환경학회:학술대회논문집
• /
• 한국지하수토양환경학회 2004년도 총회 및 춘계학술발표회
• /
• pp.354-357
• /
• 2004

The addition of oxygenates to diesel fuel can significantly reduce particulate emissions. Dibutyl maleate (DBM) and tripropylene glycol methyl ether (TGME) have been identified as possible additives based on their physicochemical characteristics and performance in engine test. However, their potential environmental impacts are unknown. therefore, practical considerations in the selection of an oxygenate additives should include cost, availability, compatibility with engines and fuel, and, particularly, its overall environmental impact. This study was investigated to determine optimal condition for the analysis of potential diesel oxygenates using SPME technique with GC-FID. Four fibers were compared and CAR/PDMS fiber was found to be the most sensitive when used direct-sampling. An absorption time of 30min and a desorption time of 5min provided to be the most sensitivity. The effects of experimental parameters such as the addition of salts, agitation, absorption time, compositon on the analysis were investigated. Analytical parameter such as linearity was also evaluated.

• 대한화학회지
• /
• 제48권1호
• /
• pp.17-27
• /
• 2004

SPME-GC/MS법을 사용하여 내분비계 교란물질로 추정되는 플라스틱 가소제류를 동시에 분석할 수 있는 방법을 고안하였다. 본 연구에서 사용한 플라스틱 가소제는 dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP), benzylbutyl phthalate(BBP), diethylhexyl phthalate(DEHP), di-n-octyl phthalate(DnOP)이었다. 표준 시료에 대한 분석결과에서 검출한계(LOD)는 0.163~0.299 ng/ml, 상대표준편차는(%RSD)는 5.85~15.80이었다. 본 방법을 사용하여 한강, 금강, 낙동강 및 섬진강에서 채취한 시료를 분석한 결과, DBP와 DEHP 만이 4대강 모두에서 미량 검출되었으며, DBP와 DEHP의 농도는 각각 0.192~1.270 ng/ml 및 0.077~1.102 ng/ml 범위를 보였다.

• Food Science and Biotechnology
• /
• 제18권4호
• /
• pp.895-899
• /
• 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
• /
• 제14권2호
• /
• pp.238-241
• /
• 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.

• 한국대기환경학회지
• /
• 제24권3호
• /
• pp.357-366
• /
• 2008

In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

• 한국식품과학회지
• /
• 제32권3호
• /
• pp.507-512
• /
• 2000

고품질 둥굴레차의 제조를 위한 기반연구로서 solid-phase microextraction(SPME)을 이용한 headspace 방법에 의해 볶음 전 중자(steaming) 여부에 따른 둥굴레차의 향기성분 특성을 비교하였다. SPME fiber에 대한 향기성분의 흡착조건은 $60^{\circ}C$에서 30분이 적합하였고, 무중자 및 중자(120분)된 시료를 $130^{\circ}C$에서 15분간 볶음 처리하여 분석 GC chromatogram에서는 40여 종의 peak가 분리되었고, 전반적인 pattern은 유사하였으나 서로 상이한 peak특성이 관찰되었다. 분리된 성분들을 GC-MS와 retention time 비교에 의해 25종을 동정하였으며, 무중자 볶음처리 둥굴레는 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, 2,5-di-methyl-4-hydroxy-3(2H)-furanone, 2-acetyl-1-pyrroline 등의 pyrazine류 함량이 중자 후 볶음 둥굴레보다 높게 나타나 둥굴레의 고유한 향과 맛에 큰 영향을 미칠 것으로 추정되었다. 특히 중자 후 볶음 처리한 둥굴레의 경우에는 acetic acid(8.17%)와 hexanoic acid(5.43%)의 함량이 무중자 시료(2.40%와 2.00%)보다 높게 나타났다.

• 한국환경과학회지
• /
• 제22권12호
• /
• pp.1539-1549
• /
• 2013

The purpose of this study is to compare the sampling methods for monitoring indoles (phenol, p-cresol, indole and skatole) in airs of swine facility. As the collecting methods of indoles in air, Tenax-TA adsorption tube and solid phase microextraction (SPME) were examined. For the preparation of calibration curves of indoles concentrated in Tenax-TA, the standard indoles solutions were spiked in each of Tenax-TA tubes and thermally desorbed (ATD) into a gas chromatograph combined with mass detector (GC/MS). And for the preparation of calibration curves by SPME, indoles in the standard gaseous solution prepared by evaporating the aqueous solution that contained indoles into a polyester sampling bag were extracted with SPME fiber and subsequently analyzed by the GC/MS. Two sampling methods were evaluated for extracting indoles present in swine building environments. Results indicated that the SPME method using Polydimethylsiloxane/ Divinylbenzene (PDMS/DVB) fiber was more effective than Tenax-TA method in extracting indoles. The gas chromatographic analysis showed that the linearities of calibration curves and detection limits were useful for detection of indoles in swine airs. The field tests also showed that considerably different levels of indoles were present in various parts of the swine building.