Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
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Comparison of Solid Phase Microextraction-Gas Chromatograph/Pulsed Flame Photometric Detector (SPME-GC/PFPD) and Static Headspace-Gas Chromatograph/Pulsed Flame Photometric Detector (SH-GC/PEPD) for the Analysis of Sulfur-Containing Compounds

Solid phase microextraction-gas chromatograph/pulsed flame photometric detector(SPME-GC/PFPD)와 static headspace-gas chromatograph/pulsed flame photometric detector(SH-GC/PEPD)를 이용한 황 함유 화합물들의 분석 방법 비교

  • Yang, Ji-Yeon (Department of Food and Nutritional Sciences, Ewha Womans University) ;
  • Kim, Young-Suk (Department of Food and Nutritional Sciences, Ewha Womans University)
  • Published : 2005.10.31
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Abstract

Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

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.

Keywords

References

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