딸기의 휘발성 향기성분의 초임계 유체 추출

이해창(Hae-Chang Lee),서혜영(Hye-Young Seo),신동빈(Dong-Bin Shin),박용곤(Yong-Kon Park),김윤숙(Yoon-Sook Kim),지중룡(Joong-Ryong Ji),최희돈(Hee-Don Choi) 한국식품과학회 2009 한국식품과학회지 Vol.41 No.6

SFE법을 이용하여 딸기의 휘발성 향기성분을 추출하기 위한 시료의 적정 전처리 및 SFE 작동조건을 검토하였으며, SDE법 및 SE법 등의 추출방법과 휘발성 향기성분 조성을 비교하였다. 딸기 생시료, 동결건조시료, 그리고 생시료에 celite를 30, 70%를 혼합하여 제조한 시료를 이용하여 SFE 처리후 향기성분을 분석한 결과, 생시료에 celite를 70% 첨가하는 방법이 향기성분을 추출하는데 가장 효과적인 것으로 나타났다. 온도(40, 55℃)와 압력(3,000, 6,000 psi)을 달리하여 SFE 처리한 결과, 3000 psi, 55℃ 조건에서 alcohol류와 acid류의 추출효율이 증가하였으며, γ-dodecalactone의 함량도 3배 정도 높은 수준으로 나타났다. SDE법, SFE법 및 SE법 등의 추출방법별 딸기의 휘발성 향기성분을 분석한 결과, SFE법은 SDE법에 비해 추출한 휘발성 향기성분의 종류는 적지만 추출량이 비슷하면서 열분해 및 열변성이 발생하지 않아 딸기 고유의 향기에 가까운 향기패턴을 나타내었으며, 기호적으로 우수한 acid류가 다량 함유된 향기성분을 추출하기에 적합한 것으로 나타났다. In order to optimize the supercritical fluid extraction (SFE) conditions of volatile components from the strawberry, we conducted an evaluation of the sample preparation and SFE operating conditions. The analysis of the volatile components extracted by a variety of sample preparation protocols led to the identification of 30, 26, 30, and 34 volatile components in fresh, freeze-dried, 30% celite and 70% celite treatments, respectively. The 70% celite treatment was the most effective in extracting the volatile components from strawberry via SFE. Analysis of the volatile components extracted by a variety of SFE operating conditions yielded identifications of 34, 35, 34, and 35 volatile components at 3,000 psi (40, 50℃) and 6,000 psi (40, 50℃), respectively. The extraction yield of alcohols and acids, and the total volatile component contents, were highest under conditions of 3,000 psi and 55℃. Volatile components from the strawberry were extracted via SFE, simultaneous steam distillation and extraction (SDE), and solvent extraction (SE). The analysis of the volatile components extracted via different extraction methods resulted in the identification of 56, 34, and 32 volatile components in the SDE, SFE, and SE extracts, respectively. The total volatile component contents identified in the SDE, SFE, and SE extracts were 20.268±1.144, 21.627±1.215 and 2.476±0.177 mg/kg, respectively. The SFE extract evidenced higher contents of sweet flavors such as 2-methylbutanoic acid, 2-methylpropanoic acid, and hexanoic acid than the SDE and SE extracts. SFE proved to be the most appropriate method for the extraction of fresh volatile components from the strawberry.

Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

서혜원,Hye Hyun Yoo,Young-Hoon Kim,Jin Hong,신윤용 사단법인 한국질량분석학회 2019 Mass spectrometry letters Vol.10 No.1

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Sepa-ration was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction moni-toring. The calibration range was 1-100ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Simultaneous Quantitative Determination of Nine Hallucinogenic NBOMe Derivatives in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry

Seo, Hyewon,Yoo, Hye Hyun,Kim, Young-Hoon,Hong, Jin,Sheen, Yhun Yhong Korean Society for Mass Spectrometry 2019 Mass spectrometry letters Vol.10 No.1

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

Comparison of SDE and SPME for the analysis of volatile compounds in butters

Yang Liu,Yunna Wang,Dongdong Yuan,Yan Li,Liebing Zhang 한국식품과학회 2020 Food Science and Biotechnology Vol.29 No.1

The current study aimed to compare the effectiveness of two extraction techniques, namely simultaneous distillation–extraction (SDE) and solid-phase microextraction (SPME), in evaluating key aroma compounds in butters. Volatile compounds’ contributions to butter flavors were evaluated employing both odor active values (OAVs) and gas chromatography olfactometry (GC-O). The results showed that the species of volatile compounds detected by the two techniques were almost the same, whereas their volatile profiles were obviously different. Using SDE method, methyl ketones took up the largest proportion of the volatile compounds, followed by fatty acids. Using SPME method, the most abundant compounds were the fatty acids, followed by lactones. More methyl ketones were detected in the SDE extract owing to lipid degradation as a consequence of the high temperature during extraction. Lactones were considered to be the key aroma compounds, especially d-decalactone, which was identified by both OAVs and GC-O.

Micro-HPLC를 이용한 조제분유 중 비타민 A,E 동시분석법 개발

윤이란 ( I Ran Yun ),최유정 ( You Jeong Choi ),이민권 ( Min Kwon Lee ),정명호 ( Byeong Hun Kim ),김병훈 한국가축위생학회 2006 韓國家畜衛生學會誌 Vol.29 No.3

Semi-micro-HPLC using a column-switching technique was developed for simul-taneous determination of vitamin A and E contents in infant formula. Vitamin A and E were extracted by PDA-HPLC with reversed phase column using organic solvent and their contents in Certified Reference Material(CRM) and infant formula were deter-mined and compared with hydrolysis method and rapid extraction. Developed method has many advantages of simple and rapid sample preparation and simultaneous deter-mination of vitamin A and E by micro-HPLC using reversed phase column.

Antioxidant Activities of Aroma Extracts in Commercially Available Red Wines in Korea

Koan Sik Woo,Geonuk Jeon,Hyang-Sik Yoon,Heon-Sang Jeong,Junsoo Lee 한국식품영양과학회 2008 Preventive Nutrition and Food Science Vol.13 No.3

The antioxidant activities of aroma extracts from commercially available red wines in Korea were evaluated. The aroma extracts of the red wines were extracted by simultaneous steam distillation. Antioxidant activity was measured by DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging activity and ABTS (2,2-azino-bis-3-ethylbenzothiazoline- 6-sulphonic acid) radical cation scavenging activity. DPPH radical scavenging activity of the aroma extracts in the red wines increased with increases in the amount of wine used for aroma extraction. Antioxidant activities of domestic wine 1, imported wine 7, and imported wine 12 were 97.16, 96.72 and 94.52%/20 mL wine by DPPH assay and 7.09, 8.07 and 7.28 mg ascorbic acid equivalents per mL wine by ABTS assay, respectively. This study demonstrates potent antioxidant activities of the aroma extracts of commercially available red wines in Korea.

Antioxidant Activities of Aroma Extracts in Commercially Available Red Wines in Korea

Woo, Koan-Sik,Jeon, Geon-Uk,Yoon, Hyang-Sik,Jeong, Heon-Sang,Lee, Jun-Soo The Korean Society of Food Science and Nutrition 2008 Preventive Nutrition and Food Science Vol.13 No.3

The antioxidant activities of aroma extracts from commercially available red wines in Korea were evaluated. The aroma extracts of the red wines were extracted by simultaneous steam distillation. Antioxidant activity was measured by DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging activity and ABTS (2,2-azino-bis-3-ethylbenzothiazoline-6-sulphonic acid) radical cation scavenging activity. DPPH radical scavenging activity of the aroma extracts in the red wines increased with increases in the amount of wine used for aroma extraction. Antioxidant activities of domestic wine 1, imported wine 7, and imported wine 12 were 97.16, 96.72 and 94.52%/20 mL wine by DPPH assay and 7.09, 8.07 and 7.28 mg ascorbic acid equivalents per mL wine by ABTS assay, respectively. This study demonstrates potent antioxidant activities of the aroma extracts of commercially available red wines in Korea.

A simultaneous microwave-assisted extraction and adsorbent treatment process under acidic conditions for recovery and separation of paclitaxel from plant cell cultures

Gun-Joong Kim,김진현 한국화학공학회 2015 Korean Journal of Chemical Engineering Vol.32 No.6

We have developed a simultaneous microwave-assisted extraction and adsorbent treatment process under acidic conditions to increase the recovery and separation efficiency of the anticancer agent paclitaxel from plant cell culture. The simultaneous process under the conditions of extracting solution (90% aqueous methanol), pH 2.2, extraction time, 6min, ratio of extracting solution to biomass, 1 : 1 (v/w), extraction temperature, 40 oC, adsorbent type, sylopute, and ratio of adsorbent to biomass, 0.08 : 1 (w/w), facilitated 1.97-fold higher recovery of paclitaxel in a shorter extraction time than the conventional solvent extraction process. In addition, biomass-derived tar compounds were successfully removed by the simultaneous process alone (average removal >97%). Using the simultaneous process, the paclitaxel extraction efficiency was improved, biomass-derived tar compounds were removed, and the purification process was simplified at the same time.

추출방법에 따른 섬백리향의 휘발성 향기성분 비교

이사은 ( Sa Eun Lee ),김성문 ( Songmun Kim ),임원철 ( Won Churl Lim ),강기춘 ( Ki Choon Kang ),표형배 ( Hyeong Bae Pyo ) 대한화장품학회 2014 대한화장품학회지 Vol.40 No.2

본 연구에서는 각 추출방법에 따른 섬백리향(Thymus magnus Nakai)의 향기 성분들을 분석하여, 이를 토대로 본연의 향에 아주 가까우면서 맡기에 좋은 향으로 재현하고자 초임계유체추출법, 혼합증류법, 동시증류추출법으로 정유를 추출한 후 gas chromatography-mass spectrometry (GC-MS)로 휘발성 향기성분을 분석하였다. 그 결과 먼저 초임계유체추출법의 40 ℃ - 400 bar 조건에서 추출한 정유 성분 중 linalool (0.1%), trans-sabinene hydrate (0.9%)가 다른 조건에서 추출한 정유성분과 비교하였을 때 상대적으로 더 많이 함유되어 있었으며, 50 ℃ - 400 bar 조건에서는 borneol (3.82%), terpinen-4-ol (0.3%), caryophyllene oxide (2.2%), 50 ℃ - 300 bar 조건에서는 β-bisabolene (5.88%), 1-octen-3 -ol (0.31%), caryophyllene (2.91%), p-cymene (2.04%), γ-terpinene (0.52%), 50 ℃ - 200 bar 조건에서는 thymol (77.63%), carvacrol (5.65%)이 상대적으로 더 많이 함유되어 있는 것으로 나타났다. 혼합증류법으로 추출한 정유 성분 중에는 α-bisabolol (0.17%), caryophyllene (6.46%), cis-α-bisabolene (1.52%), β-bisabolene (20.65%)이 초임계유체추출법으로 추출한 정유 성분 보다 상대적으로 더 많이 함유되어 있는 것으로 나타났으며, 동시증류추출법을 통해서는 정유를 얻지 못하였다. 이 같은 연구 결과는 각각의 추출법을 통해서 확인된 향기 성분들을 모두 취합하여 섬백리향 본연의 향에 좀 더 가깝도록 세밀하게 재현하는데 있어 유용한 자료로 활용될 수 있을 것으로 보인다. The purpose of this study was to analyse the volatile components of Thymus magnus Nakai extracted by different extraction methods and reproduce scent close to original plant based on the results. For this purpose, the essential oil of T. magnus was extracted by supercritical fluid extraction (SFE), water and steam distillation (WSD) and simultaneous steam distillation and extraction (SDE) methods. The compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GC-MS). Consequently, linalool (0.1%) and trans-sabinene hydrate (0.9%) contents in the essential oil extracted by SFE method of 40 ℃ - 400 bar condition were relatively higher than compositions of the essential oil extracted by different conditions. The contents of borneol (3.82%), terpinen-4-ol (0.3%) and caryophyllene oxide (2.2%) were relatively higher at 50 ℃ - 400 bar and the contents of β-bisabolene (5.88%), 1-octen-3-ol (0.31%), caryophyllene (2.91%), p-cymene (2.04%) and γ-terpinene (0.52%) were extracted relatively higher at 50 ℃ - 300 bar. The compositions of the essential oil extracted by SFE method of 50 ℃ - 200 bar condition contained relatively higher contents of thymol (77.63%) and carvacrol (5.65%). The contents of α-bisabolol (0.17%), caryophyllene (6.46%), cis-α-bisabolene (1.52%) and β-bisabolene (20.65%) in the essential oil extracted by WSD method were relatively higher than compositions of the essential oil extracted by SFE method, and by SDE method we couldn't obtained essential oil. The results of this study could be utilized to reproduce scent close to original scent of T. magnus.

Simultaneous treatment (cell disruption and lipid extraction) of wet microalgae using hydrodynamic cavitation for enhancing the lipid yield

Lee, Ilgyu,Han, Jong-In Elsevier 2015 Bioresource technology Vol.186 No.-

<P><B>Abstract</B></P> <P>Simultaneous treatment (combining with cell disruption and lipid extraction) using hydrodynamic cavitation (HC) was applied to <I>Nannochloropsis salina</I> to demonstrate a simple and integrated way to produce oil from wet microalgae. A high lipid yield from the HC (25.9–99.0%) was observed compared with autoclave (16.2–66.5%) and ultrasonication (5.4–26.9%) in terms of the specific energy input (500–10,000kJ/kg). The optimal conditions for the simultaneous treatment were established using a statistical approach. The efficiency of the simultaneous method was also demonstrated by comparing each separate treatment. The maximum lipid yield (predicted: 45.9% and experimental: 45.5%) was obtained using 0.89% sulfuric acid with a cavitation number of 1.17 for a reaction time of 25.05min via response surface methodology. Considering its comparable extractability, energy-efficiency, and potential for scale-up, HC may be a promising method to achieve industrial-scale microalgae operation.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Simultaneous treatment using HC was proposed to enhance the lipid yield. </LI> <LI> Optimal conditions for lipid extraction from <I>Nannochloropsis salina</I> were determined. </LI> <LI> HC was energy-efficient compared with autoclaving and ultrasonication. </LI> </UL> </P>