• Analytical Science and Technology
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• v.25 no.5
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• pp.292-299
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• 2012

GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.

• Korean Journal of Agricultural Science
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• v.36 no.2
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• pp.219-224
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• 2009

Two functional modified-butterfats (MF668 and MF866) were synthesized with two blends (6:6:8 and 8:6:6, w/w%) of anhydrous butterfat (ABF), palm stearin (PS) and flaxseed oil (FSO, omega-3) via lipase-catalyzed interesterification reaction. Their flavor characteristic was investigated using electronic nose and SPME-GC/MS analysis. Each flavor pattern of ABF, FSO, MF668 and MF866 was significantly discriminated with first principal component score of 95.16% in PCA plot. In functional modified-butterfats analyzed with SPME-GC/MS, various volatile compounds such as aldehydes, ketones, acids, and alkanes were detected.

• Analytical Science and Technology
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• v.14 no.2
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• pp.109-114
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• 2001

The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry(GC-MS). Flavor-related compounds were estragole pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin. More than on of the flavor-related compounds were detected in the range $0.001-1.3{\mu}g/g$ from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%.

• Proceedings of the Korea Air Pollution Research Association Conference
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• 2001.11a
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• pp.344-345
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• 2001

대기 중에는 ppb 수준의 매우 미량으로 많은 VOC 성분이 존재하고 있어 이를 효과적으로 신속하고 적은 비용으로 분석할 수 있는 분석할 필요성이 커지고 있다. 그러므로, 본 연구에서는 대기중의 VOC성분을 SPME-GC/MS법을 이용하여 효율적으로 분석하기 위한 분석법을 개발하고자 하였다. 유해성이 큰 halocarbon, aromatic, haloaromatic V()Cs 42 종(USEPA TO-14)과, 오존을 유발시키는 오존전구물질 VOCs 53 종, 국내 규제 VOCs 33종, 그리고 악취물질(국내 8종 포함 일본 악취물질 22종)을 전부 포함하는 111종의 VOC를 SPME-GC/MS를 이용하여 신속하게 정성, 정량분석할 수 있는 방법을 확립하고저 하였다. (중략)

• Proceedings of the Korean Society for Food Science of Animal Resources Conference
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• 2006.05a
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• pp.209-213
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• 2006

본 연구는 재래흑돼지와 개량종 돼지 가열육의 SPME-GC/MS와 전자코를 이용한 휘발성 향기 성분 및 향기 패턴 비교를 구명하고자 실시하였으며, 평균 생시 체중이 70 kg인 재래흑돼지(거세돈) 5두와 103 kg인 개량종 돼지($Landrace{\times}Yorkshire$,거세돈) 5두를 도축후 뒷다리 부위를 시료로 이용하였다. SPME-GC/MS를 이용한 휘발성 향기 성분에서 6-mehtyl-1-heptanol이 재래흑돼지육에서만 검출되었고, 1-octen-3-ol과 benzaldehyde가 재래흑돼지육이 개량종 돼지육보다 유의적으로 높았다(p<0.05). 전자코의 PCA에 의한 향기 패턴은 두 품종간에 큰 차이를 보이지 않았다. 따라서 재래흑돼지 가열육이 개량종 돼지 가열육보다 높은 6-mehtyl-1-heptanol, 1-octen-3-ol, benzaldehyde를 가졌으며, SPME-GC/MS와 전자코에 의해 품종이 다른 가열 돈육의 휘발성 향기 성분과 패턴을 성공적으로 분별하였다.

• Mass Spectrometry Letters
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• v.4 no.1
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• pp.18-20
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• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• YAKHAK HOEJI
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• v.54 no.6
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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.

• Analytical Science and Technology
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• v.14 no.6
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• pp.471-475
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• 2001

Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

• Analytical Science and Technology
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• v.20 no.6
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• pp.488-495
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• 2007

A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.

• Korean Journal of Food Science and Technology
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• v.48 no.5
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• pp.430-436
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• 2016

Solid phase microextraction and gas chromatography-mass spectrometry (SPME/GC-MS), electronic nose, and electronic tongue were used to characterize the sensory profiles of cider vinegars from Korea (K1-2), China (C1-2), Japan (J1-2), and US (U1-2). SPME-GC/MS detected acetic acid as the common volatile compound in all vinegars, in addition to isovaleric acid, octanoic acid, and phenethyl acetate. Acids and acetic esters were the major components of Korean and US vinegar samples, respectively. Chinese vinegars had high ethyl acetate content, while Japanese samples were characterized by a low content of acetic acid. Principal component analysis (PCA) pattern provided a clear categorical discrimination of Chinese vinegars by E-nose and E-tongue analyses. The instrumental sensory scores and the taste attributes for flavor ($r^2=0.9431$), sourness ($r^2=0.9515$), and sweetness ($r^2=0.8325$) were highly correlated. Therefore, SPME/GC-MS, E-nose, and E-tongue analyses may be useful tools to discriminate the sensory profiles of cider vinegars of different origins.