Chrysanthemum boreal, C. indicum, and C. indicum var. albescens are well-known wild Chrysanthemum species used for traditional medicine in Korea. In this study, volatile compounds from three wild Chrysanthemums were identified according to four different flowering stages and analyzed using HS-SPME-GC-MS to determine the temporal variation of the volatiles. As a result, 132, 151, and 142 peaks were identified from C. boreale, C. indicum, and C. indicum var. albescens, respectively. Furthermore, 70 out of 132 peaks were identified in C. boreale with a matching ratio of >90% from library search. In addition, 85/151 and 76/142 peaks were identified from C. indicum and C. indicum var. albescens. Forty-nine volatile compounds were found commonly in all three wild Chrysanthemums through all four different flowering stages. However, six, seven, and five unique compounds were detected only in C. boreale, C. indicum, and C. indicum var. albescens, respectively. One hundred volatile compounds were selected for multivariate analysis considering volatile compounds overlapped with each other. The one-way ANOVA (p < 0.05) detected significant differences from 77 out of 100 volatile compounds. In addition, PLS-DA showed the different profiles of volatile compounds according to four different flowering stages in each wild Chrysanthemum. PC1 of each Chrysanthemum accounted for 45.8 56.9, and 11.9% in C. boreale, C. indicum, and C. indicum var. albescens, respectively. PC1 of C. boreale and C. indicum clearly separated the BF stage and the other three stages. Conversely, PC1 of C . indicum var. albescens showed a difference in the composition of volatile compounds between the BF/BO and HO/FO stages. In addition, the different profiles of volatile compounds could be visualized using a heatmap from three wild Chrysanthemums according to four different flowering stages. This study will help improve particular volatile compounds in three wild Chrysanthemums both in quality and quantity.

본 연구는 HS-SPME/GC-MS 방법과 화학계량학 (chemometrics) 분석으로 차의 등급과 품질 판단의 가능성을 실험한 연구이다. HS-SPME/GC-MS 방법으로 녹차, 재가공차 (화차), 홍차 및 등급별 향기를 분석했고, 주성분분석, 부분최 소제곱회귀분석 등 chemometrics와 관능 평가 결과를 결합하여 차의 종류와 등급 예측 판단을 진행하였다. 주성분분석결과는 차의 종류 판별에 양호한 결과를 내었고, 녹차 Y1(X)=- 7.138-4.094X1-7.876X2, 재가공차(화차) Y2(X)=-7.291- 2.059X1+8.157X2, 홍차 Y3(X)=-3.060+4.022X1+0.746X2 판별 함수를 얻었으며 교차검증 및 식별 인자 모두 100%의 정확률 에 도달했다. GC-MS 시그널과 차의 등급에서 부분최소제곱 회귀분석을 진행하고, 관능 평가 결과와 함께 차의 종류 및 등급 예측 판단을 진행하였다. 예측값과 실제값의 상관성은 각각 대불용정 0.9056, 재스민차 0.8855, 운남홍차 0.9527, 기문 홍차 0.9710으로, 재스민차의 값이 약간 낮은 외에 모두 0.9 이상의 의미있는 결과를 보였다. GC-MS와 화학계량학 분석 으로 차의 등급과 품질 판단 연구를 진행하고, 차의 종류 식별 함수와 등급 예측 모형 수립은 차의 종류와 등급 판별에 참고 가치가 있다는 결론을 내었다.

The change in volatile compound composition of three wild chrysanthemum species (Chrysanthemum boreale, C. indicum, and C. indicum var. albescens) was identified and analyzed according to four flowering stages using HS-SPME-GC-MS (headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry). The top five compounds of each flowering stage were selected because those main compounds accounted for 43.25%, 44.14%, and 54.20% of the total relative content of volatile compounds from C. boreale, C. indicum, and C. indicum var. albescens, respectively. Nine compounds (1S-α-pinene, α-thujone, chrysanthenone, umbellulone, thymol, caryophyllene, germacrene D, α-zingiberene, and α-patchoulene) in C. boreale were ranked in the top five compounds through the whole flowering stages. In C. indicum, camphene, eucalyptol, camphor, umbellulone, bornyl acetate, caryophyllene, β-farnesene, germacrene D, and α-zingiberene were ranked in the top five compounds. However, only five compounds (camphor, bornyl acetate, β-farnesene, germacrene D, and α-zingiberene) were ranked in C. indicum var. albescens showing a more stable composition rather than C. boreale and C. indicum. Flowerheads of three wild Chrysanthemums showed a different profile of volatile compounds according to different flowering stages, varying compositions, and relative content in the top five volatile compounds. This study illustrates how main volatile compounds in wild chrysanthemums change dynamically during the flowering regarding compositions and their relative contents, suggesting that it should provide a useful index for harvesting or blending certain target compounds from wild chrysanthemums.

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.

In this study, the calibration characteristics of six new odorant VOCs along with two reference compound were evaluated based on GC-MS (SIM). For the proper evaluation of the GC/MS method, calibration of 7 VOCs were made both by the SPME and direct injection (DI). The minimum detection limit (MDL) of those VOC determined by SPME method fell in the range of 0.31∼0.38 ppb while those of DI from 6.18∼14.3 ppb. The analytical performance of our SPME/GC-MS method was compared against those tested previously by other study groups. Although more efforts are needed to establish the reliability of our SPME/GC-MS method, the method adapted in this study can be recommended as one of the standard methods for the analysis of the target VOCs in this study to settle formal experiment methods.

In this study, the performance of fast gas chromatography system was evaluated using VOC standards prepared in both liquid and gaseous phase. When the liquid‐phase VOC standards were analyzed by both direct injection and HS‐SPME method, all the chromatographic separation was completed within 4 minutes. The calibration experiments were conducted further using gaseous standard of BTX. The calibration results derived by direct injection method generally showed good linearities, regardless of phases, while it was not the case for HS‐SPME method. In case of liquid‐phase standard, MDL values for direct injection and HSSPME method were calculated in the range of 0.07~0.19 to 0.63~3.76 ng, respectively. In contrast, MDL values for gaseous standard were 0.27~0.45 and 1.94~6.90, respectively. The reproducibility of our method, when expressed in terms RSE, showed above 5 %. When the sensitivity of different techniques is compared, the calibration slope values of BTX decreased on the order: direct injection of liquid‐phase standard > HSSPME method of liquid‐phase standard > direct injection of gaseous standard > HS‐SPME method of gaseous standard. Although fast GC is very efficient to reduce the total running time significantly, extended studies are desirable to improve its reproducibility.

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 α-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.

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.

Background : Matricaria recutita and Dendranthema indicum are known to have effects such as antioxidant and antihypertensive effects, and they are used as processed food materials. Therefore, it is necessary to examine the possibilities as a natural material for cosmetics. This study was carried out to analyze the volatile flavor components of flowers during cultivation in order to examine the possibility of cosmetics using M. recutita and D. indicum. Methods and Results : This experiment was carried out from April to October, 2017 at Unbong-eup (500 m above sea level) in Namwon, Jeollabuk-do. M. recutita and D. indicum were planted in late May. Then, flowers were collected in October and volatile flavor components were analyzed by Solid Phase Micro Extraction (SPME) method. Samples of flowers for component analysis were weighed in 0.4 g each and placed in a 20 ㎖ vial. GC/MS was used with Agilent Technologies 7890A/5975C (Agilent, USA). Column and carrier gas were DB-5MS (30 m × 0.25 ㎜ × 0.25 ㎛) and helium gas, respectively. As a result of the analysis of M. recutita flowers, we identified a total of 24 components. The major flavor components were mono terpenes and ketones. The main compounds were β-ocimene (24.08%), artemisia ketone (22.82%), γ-terpinene (16.65%), cis-3-hexenyl isovalerate (3.92%), artemisiatriene (3.72%) and O-cymene (3.44%). As a result of analyzing the composition of D. indicum flower, we identified 33 kinds of ingredients. The major flavor components were monoterpenes and sesquiterpenes. The main compounds were sabinene (19.67%), trans-oiperitol (13.22%), α-phellandrene (10.05%), myrcene (7.53%), cineole (4.36%), α-terpinene (3.60%) and trans-ocimene (3.57%). Conclusion : We identified 24 flavor components and 33 flavor components in flower of M. recutita and D. indicum, respectively. Eight of the identified or estimated compounds were common to both samples. The reason why the flavor components kinds of M. recutita flowers were few was thought to be due to the influence of collection time. The main flowering period of M. recutita and D. indicum were May and October, respectively, but the use of the samples collected in October seemed to have influenced.

This study was conducted to compare the volatile flavor compounds of Artemisia annua L. after extraction by simultaneous steam distillation extraction (SDE) and solid-phase micro extraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis. Via SDE and SPME processes, 79 (1,254.00 mg/kg) and 39 (488.74 mg/kg) compounds were identified respectively. The compounds extracted by SDE included 27 alcohols, 13 aldehydes, 22 hydrocarbons, 3 esters, 12 ketones, 1 oxide and 1 N-containing compound, on the other hand, using the SPME method, 7 alcohols, 5 aldehydes, 1 ester, 18 hydrocarbons, 7 ketones, and 1 oxide were extracted. The major volatile flavor compounds of Artemisia annua L. isolated by the two methods were caryophyllene oxide, -caryophyllene, camphor, -selinene, -muurolene, 1,8-cineol, (E)-pinocarveol and pinocarvone. β β γ The sesquiterpene named caryophyllene oxide was the most abundant volatile flavor compound with relative contents of 234.16 mg/kg and 195.44 mg/kg obtained by the SDE and SPME methods, respectively. Among the identified volatiles, sabinene, β-pinene, α-terpinene, γ-terpinene, yomogi alcohol, myrtenol, (Z)-nerolidol, p-cymen-8-ol and eugenol were detected by the SDE method only while (E)-anethole and α-cubebene were detected by the SPME method only. This study confirmed that the composition and contents of the volatile flavor compounds vary between different extraction methods. More volatile flavor compounds were identified using the SDE method than the SPME method.

A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. 50/30 ㎛ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to 0.15 ㎍/L for VFAs and from 0.12 to 0.28 ㎍/L for indoles and the correlations observed (R2) were 0.975～1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

The purpose of this study is to compare the sampling methods for monitoring indoles (phenol, p-cresol, indole and skatole) in airs of swine facility. As the collecting methods of indoles in air, Tenax-TA adsorption tube and solid phase microextraction (SPME) were examined. For the preparation of calibration curves of indoles concentrated in Tenax-TA, the standard indoles solutions were spiked in each of Tenax-TA tubes and thermally desorbed (ATD) into a gas chromatograph combined with mass detector (GC/MS). And for the preparation of calibration curves by SPME, indoles in the standard gaseous solution prepared by evaporating the aqueous solution that contained indoles into a polyester sampling bag were extracted with SPME fiber and subsequently analyzed by the GC/MS. Two sampling methods were evaluated for extracting indoles present in swine building environments. Results indicated that the SPME method using Polydimethylsiloxane/ Divinylbenzene (PDMS/DVB) fiber was more effective than Tenax-TA method in extracting indoles. The gas chromatographic analysis showed that the linearities of calibration curves and detection limits were useful for detection of indoles in swine airs. The field tests also showed that considerably different levels of indoles were present in various parts of the swine building.

This study was conducted to investigate changes in the main volatile flavor components of oriental melon during the process of alcohol fermentation via SPME (solid phase micro extraction). The flavor components of oriental melon were shown to have mainly included melon and green flavors. The green flavor was identified to be nonanal, 1-butanol, 1-octen-2-ol and benzene, and its relative concentration was shown to be 16.66%. The nonanal concentration was shown to have been reduced among the green-flavor components, but no significant change in remaining components was observed. Mainly, sweet flavor tended to increase, and the relative concentration of benzene was particularly shown to have increase by 25.58%, accounting for the highest relative concentration. The amount of green-flavor components, except for 1-butanol, was shown to have significantly decrease after alcohol fermentation. Then, no component of green-flavor, which causes an offensive smell, was found during fermentation and aging. Meanwhile, the volatile flavor components, which are consist of acids, were shown to have been produced during alcohol fermentation. In particular, octanoic acid, which causes off-flavor, was shown to be 60.99%, a very high relative concentration during the aging stage. In addition, acetic acid with a pungent sour flavor tended to be produced. A further study on the improvement of flavor in the production of oriental melon wine is required.