Earticle

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.

SDE 및 SPME를 이용하여 계피로부터 추출한 휘발성 향기성분을 GC/MSD 분석한 결과 terpenes 20종, alcohol 3종, carbonyl 5종, esters 2종으로 총 30개의 휘발성 성분을 확인하였다. 이들 중 trans-cinnamaldehyde (86.4%), cis-cinnamaldehyde(0.9％), hydrocinnamaldehyde (0.1%) 등의 carbonyl 화합물이 peak area% 기준으로 약 88.2%로 계피 중 대부분을 차지하는 것으로 나타났다. 또한 식물체의 향기성분 분석에 많이 이용되는 SPME fiber 4종류를 비교 분석한 결과 terpen류 화합물들은 PDMS fiber에서 추출효율이 가장 좋았으며, cinnamyl alcohol과 같은 다소 극성인 화합물의 경우 DVB/CAR/PDMS fiber와 PA fiber에서 추출 효율이 가장 좋은 것으로 나타났다. SPME법에서 최적 조건을 설정하기 위해 추출온도와 추출시간을 달리하면서 비교 분석한 결과 copaene, murolene, cadinene, cis-cinnamaldehyde 등의 area% 값은 온도와 시간이 커질수록 증가한 반면에 trans-cinnamaldehyde의 area% 값은 감소하였다.

The volatile components of cinnamon bark were extracted by using different isolation methods, simultaneous distillation extraction (SDE) and solid phase microextraction (SPME). Then the volatile components were analyzed by gas chromatography(GC) and mass selective detector(MSD). 30 compounds were identified in cinnamon bark. In SPME technique, several factors influencing the equilibrium of the aroma compounds between sample and SPME fiber was taken into account, including the kind of SPME fiber, extraction temperature and extraction time. Four different SPME fibers were tested, namely polydimethylsiloxane (PDMS), poly acrylate(PA), divinyl- benzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and carbowax/divinylbenzene(CW/DVB). Among these SPME fiber, PDMS coating fiber showed the best results. The profile of volatile compounds of cinnamon bark at different extraction temperature and extraction time were investigated by 100$\mu\textrm{m}$ PDMS fiber.

This study was carried out to find the possibility of use of Solid Phase Microextraction(SPME) for extracting the volatile aroma compounds in the five aromatic plants (Agastache rugosa O. Kuntze, Mentha arvensis Linne, Thymus quinquecostatus Celakovsky, Elsholtzia splendens Nakai, Schizonepta tenuifolia Briquet) belongs to the Labiatae. In the result of the analysis, the volatile aroma compounds were mainly composed monoterpene alcohol (Iinanol, menthol, α-terpineol, borneol), monoterpene ketone (limonene, menthone) and sesquiterpene (trans-caryophyllene,δ-cadinene). The volatile aroma compounds of Agastache rugosa O. Kuntze and Mentha arvensis Linne were extracted by SPME more identified than the SDE. However, Schizonepta tenuifolia Briquet more identified by the SDE and in Elsholtzia splendens Nakai similar to the SDE. Especially, the SPME showed the sesquiterpene contents was more than the SDE. The major volatile aroma compounds were difference but the composition of those between the SPME and the SDE showed no difference. Within the results, the SPME showed the most convenient and a rapid extraction method to analysis of the volatile aroma compounds.

The volatile components of Pinus densiflora needles were studied by gas chromatography-mass spectrometry(GC-MS), using seven kinds of solid phase microextraction (SPME) fibers, seven in SPME fibers: 100 ${\mu}m$ PDMS, 65 ${\mu}m$ PDMS/DVB, 65 ${\mu}m$ SF-PDMS/DVB, 85 ${\mu}m$ PA, 75 ${\mu}m$ CAR/PDMS, 65 ${\mu}m$ CW/DVB and 50/30 ${\mu}m$ DVB/CAR/PDMS fibers. A total of 40 components were identified by using the seven different SPME fibers. The identified components were classified, according to their functionalities, as follows: 26 hydro-carbons, 7 alcohols, 4 carbonyl compounds, and 3 esters. The major volatile components of Pinus densiflora needles identified by these SPME fibers were $\alpha$-pinene ($1.7\~21.7\;{\mu}g/g$), $\beta$-myrcene ($2.0\~20.1\;{\mu}g/g$), $\beta$-phel-landrene ($4.6\~22.8\;{\mu}g/g$), $\beta$-caryophyllene ($6.7\~26.0\;{\mu}g/g$) germacrene D ($1.1\~11.9\;{\mu}g/g$). In the comparison of the seven SPME fibers, PDMS appeared to be the most suitable fiber for the analysis of hydrocarbon compounds and CAR/DPMS, PDMS/DVB, CW/VB and DVB/CAR/PDMS are shown to be optimal for analysis of the alcohols and carbonyl compounds.

기체크로마토그래프-질량분석법(GC/MS)의 Scan 및 SIM mode 동시 분석법을 이용하여 25종의 유기인계 농약성분을 선택적으로 분석하였으며 추출은 고체상미량 추출법으로 Oasis HLB 카트리지를 사용하였다. 전자충격으로 분석대상 화합물을 이온화시켰으며 Scan mode와 3개의 특징 이온을 이용한 SIM mode로 각각의 크로마토그램을 얻었다. GC/MS의 SIM mode의 검출정도는 Scan mode 보다 좋으나 특정 목적 성분이외는 어떤 정보도 얻을 수 없는 단점이 있기 때문에 Scan mode를 동시에 얻음으로서 이 러한 단점을 보완할 수 있었으며 SIM mode를 이용하여 25종의 유기인계 농약성분에 대하여 시험법에 대 한 유효화를 실시하였다. 혈액에서 25종의 유기인계 농약 성분의 회수율은 62.8% ~ 98.0%였으며 검출한계 및 정량한계는 각 각 5 ng/mL ~ 10 ng/mL 및 10 ng/mL ~ 20 ng/mL로 나타났다. 직선성은 20 ng/mL의 농도 로부터 유기인계 농약의 성분에 따라 250 ng/mL ~ 2500 ng/mL에서 r2 = 0.99 이상의 직선성을 보였으며 시험 간 및 시험 내의 정확도와 정밀도가 유효화 조건을 충족하였다.

This study described a specific and sensitive method for the determination of 25 organophosphorus pesticides in blood, using a rapid solid-phase extraction(SPE) procedure with Oasis HLB cartridges and gas chromatography-mass spectrometry in synchronous scan and selective ion monitoring(SIM) modes. The ionization was carried out by electron impact and acquisition in scan and SIM mode identifying three specific ions per component. Scan GC/MS analysis is a commonly employed data collection mode for pesticides to acquire both qualitative and quantitative information and SIM analysis provides more sensitivity than the scan mode does, but does not give any information regarding non-target analytes. So combining these two analysis modes makes a more powerful analysis method that can give synchronously both qualitative and quantitative information. Extraction recoveries were satisfactory and ranged between 62.8 and 98.0% in blood. Limits of detection (LODs) ranged from 5 to 10 ng/mL and limits of quantitation (LOQs) ranged from 10 to 20 ng/ mL in blood. An excellent linearity was observed, r2> 0.99, from 20 up to 250-2500 ng/mL for the components of organophosphorus pesticides. Intra- and inter-assay precision and accuracy were satisfactory for the most of 25 organophosphorus pesticides analyzed.

각각의 황 함유 화합물의 표준곡선을 그렸을 때, linear range의 범위는 부터 까지의 범위를 보였다. Dimethyl trisulfide가 가장 작은 limit of detection(LOD) 값과 가장 넓은 linear range 를 보이는 반면, methional은 가장 큰 LOD 값과 가장 좁은 linear range를 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.

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 . 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.

본 실험에서는 시판중인 우유 4종을 대상으로 static headspace, purge and trap 및 SPME의 세 가지 향기성분 추출방법을 이용하여, GC/MS로 각각의 향기성분을 분석하였다. Purge and trap법을 이용한 분석법으로 가장 많은 종류의 성분을 분석할 수 있었으며, 향기성분의 추출효율이 가장 좋았다. SPME법은 간단한 장비로 신속하게 향기성분을 포집할 수 있는 장점이 있으며, 추출 효율 또한 뛰어나 효율적인 향기성분 분석방법으로 이용이 가능하였다. 4종의 시판우유 중에서 검출된 향기성분은 대체적으로 큰 차이를 나타내지 않았으나, 다소의 양적차이를 나타내었다. 검출 된 성분은 주로 acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone 등의 케톤류, pentanal, 2-methylbutanal, hexanal, benzaldehyde 등의 알데하이류 및 dimethyl sulfide 등의 황화합물류로써, 우유의 주요 이취성분들이었다.

Volatile flavor compounds in commercial sterilized milk were analyzed and identified by static headspace, purge-and-trap, and solid-phase microextraction (SPME) methods. About 20 volatile compounds were identified by GC/MS, and aldehydes and ketones were the most distinctive and abundant compounds. Static headspace analysis allowed the identification of only the most abundant compounds, such as acetone. Five ketones (acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone), four aldehydes (2-methylbutanal, pentanal, hexanal, benzaldehyde) and dimethyl sulfide, all of which were responsible for off-flavor in milk, were found by the purge-and-trap and SPME methods. The two methods differed little in their release of these compounds, but they yielded different amounts in the extraction.