• 한국식품조리과학회지
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• 제19권1호
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• pp.79-82
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• 2003

Volatile compounds in Elsholtzia splendens were extracted by solid phase microextraction (SPME). Two kinds of SPME fiber, carboxen/polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane (PDMS) were used to determine the selectivity of the fibers to the different flavor compounds present in the Elsholtzia splendens. Identification of volatile compounds was based on the linear retention indices (RI) and the comparison of their mass spectra with those of on-computer library. Thirty compounds were identified in the volatile compounds extracted by CAR/PDMS fiber, including 1 aldehyde, 5 alcohols, 3 hydrocarbons, 17 terpene hydrocarbons, 3 ketones and 1 miscellaneous. And 5 alcohols, 3 hydrocarbons, 18 terpene hydrocarbons, 3 ketones and 2 miscellaneouses were identified in PDMS fiber. These results suggested that the selectivity of PDMS fiber was similar to that of CAR/PDMS fiber in Elsholtzia splendens. The major volatile compounds were naginataketone and elsholtziaketone in Elsholtzia splendens.

• 한국식생활문화학회지
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• 제22권2호
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• pp.246-253
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• 2007

참나물의 잎과 줄기부위에서 가장 많이 함유하고 있는 무기 성분은 K, P, Ca, Mg 순이었으며 잎 부위가 줄기부위보다 Ca, P, Mg함유량이 약 4배 정도 많았다 전자코를 이용한 휘발성 향기성분 패턴은 신선한 참나물의 경우 제1주성분 값이 +값을, 음건한 건조 참나물은 - 값을 나타내어서 신선한 참나물과 건조한 참나물 사이에는 뚜렷한 차이를 보였고 건조방법에 따른 시료간의 구별이 가능하였다. SDE법에 의해 신선한 참나물은 aldehydes 3종, alcohols 9종, ester 4종, hydrocarbons 5종, terpen hydrocarbons 34종, ketone 1종, 기타 2종의 총 58 종이 확인되었고, 음건한 참나물은 aldehydes 4종, alcohols 7종, hydrocarbon 1종, terpen hydrocarbons 17종, ketone 1종, 기타 1종의 총 31종이 확인되었다. SDE법에 의한 신선, 음건한 참나물 모두 ${\alpha}$-selinene(37.89%, 12.59%)가 가장 많이 확인되었는데 신선할 때보다 음건한 경우 휘발성향기성분의 peak수와 peak area%가 적었다. CAR/PDMS fiber HS-SPME법에 의해 34종이 확인되었는데 aldehydes 2종, alcohols 2종, hydrocarbons 7종, terpen hydrocarbons 23종이며 myrcene(15.50%)가 가장 많이 확인되었다. PDMS fiber HS-SPME법에 의해 aldehydes 1종, alcohols 1종, hydrocarbons 2종, terpen hydrocarbons 17종으로 총 21종이 확인되었고 germacrene D(16.84%)가 가장 많았다. SDE법에 의한 경우가 SPME법보다 향기성분의 종류와 양이 많았고 HS-SPME법의 경우 CAR/PDMS fiber가 PDMS fiber 보다 더 많은 종류의 향기가 확인되었다.

• Bulletin of the Korean Chemical Society
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• 제34권1호
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• pp.139-142
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• 2013

A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

• 상하수도학회지
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• 제19권6호
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• pp.713-719
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• 2005

SPME (Soild phase microextraction) has been used in the analysis of many volatile organic compounds, such as geosmin and 2-methylisoborneol (2-MIB), trihalomethanes (THMs) in drinking water. SPME fiber is characterized by high adsorption capacity (DVB/CAR/PDMS, DVB/PDMS etc.). Although the highly active adsorption capacities of the SPME fiber are often to the chemical functional group, surface properties play a significant role in determining the surface adsorption capacities. The objectives of this study were to evaluate effect of residual chlorine on analysis of geosmin and 2-MIB. Image taken by SEM before preloaded with chlorine, the surface and porous media was almost perfect spherical shape and no clogging of pores. However, after preloaded with chlorine the surface was aggregated and pore was blocked. The recovery rate of geosmin and 2-MIB coexisting with chlorine was reduced by 35 to 62%. The recovery rate with preloaded with chlorine was reduced by 25 to 43%. The lower concentration of geosmin and 2-MIB and the higher concentration of chlorine existed in water, the lower the recovery rate was.

• 한국식품과학회지
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• 제33권1호
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• pp.153-156
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• 2001

2단계 발효로 제조한 감식초를 static headspace-GC법과 SPME-GC법으로 휘발성 성분을 각각 포집 분석하여 상호간의 특성에 대해 조사하였다. 감식초의 휘발성 성분 포집조건은 $80^{\circ}C$에서 20분간으로 설정하였으며, 감식초 휘발성 성분의 total FID response는 CW/DVB fiber를 이용한 SPME법에서 total peak area $18.18{\times}10^6$로, static headspace-GC법의 total peak area $1.35{\times}10^6$보다 현저하게 높았다. 감식초의 주된 휘발성 성분으로 acetic acid, ethyl acetate, 3-hydroxy-2-butanone, ethanol, phenethyl alcohol 등이 확인되었으며, static headspace-GC법에서는 acid류 3종, aldehyde류 3종, alcohol류 5종, ester류 8종 및 ketone류 1종이 확인되었다. SPME-GC법에서는 acid류 6종, aldehyde류 7종, alcohol류 6종, ester류 9종, hydrocarbone류 2종, ketone류 1종, 기타 3종으로, 총 34종의 휘발성 성분이 확인되었으며, benzaldehyde, phenethylacetate, phenethylalcohol 등의 비율이 headspace-GC법에 비해 높았다.

• Food Science and Biotechnology
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• 제18권3호
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• pp.579-585
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• 2009

Solid-phase microextraction (SPME) has gained widespread acceptance in sample pretreatment due to its solvent-free and easy-to-operate properties. SPME fibers are considered as a key part of SPME technique, since it primarily determines the extraction performance of the method including sensitivity, selectivity, and reproducibility. Generally speaking, target analyte with different chemical property requires fiber coating that has the best affinity towards it. Due to the lack of varieties of commercial fibers available currently, considerable efforts have been recently made to develop tailor-made fibers to fulfill increasing demands of different analysis. This paper concisely classify some SPME fiber preparation approaches such as sol-gel technology, physical deposition, molecularly imprinted technique, and their respective application in food safety analysis.

• 한국식품과학회지
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• 제37권5호
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• pp.695-701
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• 2005

각각의 황 함유 화합물의 표준곡선을 그렸을 때, linear range의 범위는 $10^2$부터 $10^4$까지의 범위를 보였다. Dimethyl trisulfide가 가장 작은 limit of detection(LOD) 값과 가장 넓은 linear range $(10^4)$를 보이는 반면, methional은 가장 큰 LOD 값과 가장 좁은 linear range$(10^2)$를 가졌다. 각 황 함유 화학물의 분자구조와 PFPD의 황 함유 화합물 분석 원칙에 영향을 받는 것으로 사료된다. 서로 다른 세 종류의 fiber를 사용시, 미세 고체상 추출법(SPME)을 사용했을 때, CAR/PDMS fiber는 가장 좋은 추출 효율을 보였고, 반대로 PDMS/DVB fiber는 가장 낮은 효율을 나타내었다. SPME 방법을 사용하면, 시료에 포함되어 있는 6개의 황 함유 화합물들 중, 최대 5개까지 분석이 가능하였다. 그러나 본 실험에서 사용하지 않은 황 함유 화합물들도 다수 동정 되었는데, 이렇게 추출과정 중 artifacts로 생성된 황 함유 화합물들은 분석 시 오차를 작용할 수 있다. 고정상 기체추출법(SH)은 SPME와 비교했을 때 더 적은 수의 황 함유 화합물을 감지해냈다. SPME와 비교 시 SH의 추출 효율은 낮았지만, artifact로 생성되는 화합물의 수는 적었다.

• 약학회지
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• 제54권6호
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• pp.429-440
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• 2010

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

• 한국축산식품학회지
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• 제29권5호
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• pp.579-589
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• 2009

This study was conducted to investigate the effects of heating, fiber type used in solid-phase microextraction (SPME, two phase vs three phase) and storage time on the volatile compounds of porcine M. longissimus dorsi (LD). Volatile compounds were measured using a gas chromatography and mass spectrometry (GC/MS) with a quadrupole mass analyzer. Among the volatile compounds identified, aldehydes (49.33%), alcohols (24.63%) and ketones (9.85%) were higher in pre-heated loins ($100^{\circ}C$/30 min), whereas, alcohols (34.33%), hydrocarbons (22.84%) and ketones (16.88%) were higher in non-heated loins. Heating of loins induced the formation of various volatile compounds such as aldehydes (hexanal) and alcohols. The total contents of hydrocarbons, alcohols, and carboxylic acids were higher in two phase fibers, whereas those of esters tended to be higher in three-phase fibers (p<0.05). Most volatile compounds increased (p<0.05) with increased storage time. Thus, the analysis of volatile compounds were affected by the fiber type, while heating and refrigerated storage of pork M. longissimus dorsi increased the volatile compounds derived from lipid oxidation and amino acid catabolism, respectively.

• 상하수도학회지
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• 제18권5호
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• pp.638-648
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• 2004

In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.