With continuous development in the field of sample preparation technology, solid phase micro-extraction (SPME) has been widely used in analytical chemistry for high extraction efficiency and convenient operation. Different materials lead to different extraction results. Among existing materials, carbon-based materials are still attracting attention from scientists due to their excellent physical and chemical properties as well as their modifiable surfaces, which could enhance the adsorption effects of SPME fiber. This review introduces the preparation methods and applications of different kinds of carbon-based material coatings on fibers. In addition, directions for future research on carbon material composites are discussed.
This study investigated the chemical composition of headspace gas from white-flowered lotus (Nelumbo nucifera Gaertner). Volatile flavor compositions of headspace from white-flowered lotus (floral leaf, stamen, flower stalk, stem) were investigated through the solid-phase microextraction method using polydimethylsiloxane-divinylbenzene fiber. The headspace was directly transferred to a gas chromatography-mass spectrometry. Sixty-three volatile flavor constituents were detected in the headspace of lotus floral leaves, and undecanoic acid (7.81%) was the most abundant component. Fifty-three volatile flavor constituents were detected in the headspace of lotus stamina, and isobutylidene phthalide (7.94%) was the most abundant component. Forty-four volatile flavor constituents were detected in the headspace of lotus flower stalks, and 3-butyl dihydrophthalide (11.23%) was the most abundant component. Fifty-nine volatile flavor constituents were detected in the headspace of lotus stems, and ligustilide (16.15%) was the most abundant component. The content of phthalides was higher in the headspace of flower stalks and stems, while alcohols and acids were the predominant compounds in lotus floral leaves.
The objective of this study was to identify the main floral scents and their relative contents in the floral organ of Nelumbo nucifera. N. nucifera flower, a traditional Chinese medicinal herb, is rich in volatile compounds. In this study, the volatile components of N. nucifera flowers were investigated by headspace solid-phase microextraction gas chromatography-mass spectrometry for each organ of the flower: petals, sepals, pistils, and stamens. In total, we identified 39 compounds, among which aliphatics were major constituents, representing more than 94% of petals and sepals volatiles, followed by sesquiterpenes representing more than 69% of pistils and stamens volatiles. Pentadecane, 1-pentadecene, 8-hexadecyne, 8-heptadecene, and β-caryophyllene characterize the scent of the N. nucifera flower. We identified 24 volatiles in petals and sepals, 25 volatiles in pistils, and 18 volatiles in stamens. Among the monoterpenes, 3-Isopropylidene-4-methylcyclohexene, isoterpinolene, p-Menth-2-en-7-ol, and methyl 2,6,6- trimethylcyclohex-1-enecarboxylate were analyzed and identified for the first time from the N. nucifera flower. This study demonstrates that N. nucifera flowers differ greatly in volatile composition depending on the floral organ of the plant.
HS-SPME법을 이용하여 한국 서남해 연안해역에서 Sea-nine 211, Irgarol 1051, Diuron과 같은 방오제의 분포 특성을 검토하였다. 반감기가 짧은 Sea-nine 211은 모든 시료채취지점 및 지역의 해수와 퇴적물에서 아주 낮은 농도 또는 검출한계 이하로 분포하였다. Irgarol 1051은 해수 및 퇴적물에서의 최고 농도가 각각 6.98μg/L, 28.50 ng/g-dry wt로 검출되었으며, 지역별 분포 특성은 나타나지 않았다. 반감기가 가장 길고 생물 농축성이 강한 Diuron은 모든 시료채취 지점에서 Sea-nine 211과 Irgarol 1051보다 높은 농도로 분포하였으며, Mo7(목포)의 퇴적물에서 최고농도(3882.22 ng/g-dry wt)로 분석되었다. Irgarol 1051과 Diuron은 조선산업단지 및 선박정박지가 위치하고 있는 지점에서 높은 농도로 분포하는 것으로 나타났다. 또한 퇴적물에서의 방오제 분포는 내만에서 외만으로 그 농도가 낮아졌다. 이러한 결과로부터 방오제는 내만에 위치하고 있는 항구나 조선산업단지로부터 오염될 가능성이 높을 것으로 판단된다.
우리나라의 고유한 향신료로 활용되고 있는 소엽의 휘발성 향기성분 분석에 적합한 solid phase microextraction(SPME) fiber를 선정하기 위하여 carboxen/polydimethylsiloxane(CAR/PDMS)과 polydimethylsiloxane(PDMS)의 2종류 fiber를 이용하여 향을 추출한 후 GC/MS로 분석하였다. CAR/PDMS fber에 소엽의 향을 흡착시켜 분석한 결과, 39종의 성분이 확인되었으며, PDMS fiber를 이용하였을 때는 20가지의 향기성분이 확인되었다. 특히 PDMS fiber를 사용하였을 때 CAR/PDMS fber를 이용하였을 때 보다 perillaldehyde (40.50%), limonene (27.32%), E,E-,α-famesene (10.22%) 및 β-caryophyllene (8.02%)의 소엽의 주요 향기성분이 선택적으로 많이 확인되었다. 따라서 방향성 식용식물인 소엽의 향기를 SPME법으로 추출할 때는 PDMS fiber가 적합하다고 판단된다.
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 fizsed silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylsiloxane (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 20 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 method, 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 showed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.
본 연구는 향기성분을 많이 포함하고 있는 꿀풀과의 대표적인 5종류를 선정하여 이들을 대상으로 소량의 시료만으로도 신속하게 분석할 수 있는 고상 미량 추출법(Solid Phase Microextraction: SPME)과 동시증류추출법(Simultaneous Distillation and Extraction : SDE)으로 향기성분을 분석하였다. 분석결과 5종류의 꿀풀과 약초의 향기성분 구성은 linanol, limonene, citral, trans-geraniol 등의 monoterpene alcohol, monoterpene aldehyde 및 ketone 과 trans-caryophyllene, δ-cadinene 등의 sesquiterpene 성분들이 주로 검출되었다. 분석결과 기존의 향기성분 연구에 많이 사용되는 동시증류추출법(SDE)과 주성분에서 대부분 유사하였으나 형개의 향기성분처럼 SPME법에서 많은 성분이 검출되지 않는 경우도 있었고 배초향, 박하의 성분처럼 SDE법에서 검출되지 않은 일부 성분도 SPME법에서 검출되기도 하였다. 이러한 결과는 SPME법은 낮은 온도에서 흡착만으로 성분의 포집이 이루어지므로 추출, 농축 등의 조작에 의한 SDE법보다 이차적인 변질이 적었기 때문으로 생각되었다. 따라서 SPME법은 열변성이 적고 소량으로 다수의 시료를 분석할 수 있어 향신약초의 품종육종 등에 사용할 수 있는 간편하고 신속한 방법이 될 것으로 생각된다.