• 한국자원식물학회:학술대회논문집
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• 한국자원식물학회 2022년도 추계학술대회
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• pp.100-100
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• 2022

Hovenia dulcis is a herbal plant, which belongs to the Rhamnaceae family and is a native of Japan, China and Korea. Its fruit stalk is called 'Jiguja' in Korea. It has been traditionally used as a medicinal plant in East Asia. It was reported to have detoxification effects on alcohol poisoning, and antioxidant, antidiabetic etc. Sample of 5 g was extracted with 50 mL of 70% EtOH. The supernatant was filtered by 0.45 ㎛ membrane filter before analysis. The UPLC system was performed on Waters alliance UPLC HSS T3 column (2.1 × 100 mm, 1.7 ㎛) with a UV detector. The gradient system was a binary eluent of 0.1% formic acid in water(A) and 0.1% formic acid in acetonitrile(B) with gradient conditions as follows: Initial, 10% B; 1 min, 10% B; 4 min, 20% B; 10 min, 25% B; 12 min, 30% B; 14 min, 90% B; 17 min, 90% B; flow rate of 0.2 mL/min. The samples were injected by 2 µL and were detected at UV 355 nm. As a result of analysis, chromatographic patterns appeared in two cases: samples analyzed for ampelopsin and myricetin, and samples analyzed for taxifolin and quercetin. Among the four compounds, the largest regional difference was found to be taxifolin.

• 분석과학
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• 제32권1호
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• pp.24-34
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• 2019

The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to $1.5{\mu}g\;mL^{-1}$, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

• Journal of Ginseng Research
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• 제42권2호
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• pp.149-157
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• 2018

Background: Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of $35^{\circ}C$. This developed HPLC-UV method provides an adequate linearity ($r^2$ > 0.999), repeatability (relative standard deviation, RSD < 2.98%), and inter- and intraday variations (RSD < 4.40%) with recovery (98.7-106.1%) of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products.

• Journal of the Korean Wood Science and Technology
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• 제44권3호
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• pp.337-349
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• 2016

본 연구는 꾸지뽕나무 열매에서 분리 및 정제한 isoflavonoid 성분에 대하여 Ultra Performance Liquid Chromatography(UPLC)을 이용하여 분석법을 개발하고 검증하고자 하였다. 꾸지뽕나무 열매를 methanol로 추출하여 n-hexane, ethyl acetate, 물 순으로 분액 후, ethyl acetate 추출물을 silica gel 컬럼과 sephadex LH-20 컬럼을 사용하여 4종의 isoflavonoid들을 분리하였다. 분리한 4종의 isoflavonoid들은 기기분석(UV-Vis spectroscopy, ESI-MS, $^1H\;NMR$, $^{13}C\;NMR$)을 통하여 alpinumisoflavone, 6,8-diprenyl orobol, 6,8-diprenyl genistein, 4'-O-methylalpinumisoflavone으로 확인 및 동정하였다. 이 성분들을 2% acetic acid 용액(용매 A)과 2% acetic acid가 함유된 MeOH 용액(용매 B)을 기울기 이동상으로 하여 $C_{18}$ 컬럼이 장착된 UPLC로 분석하였다. 분석 조건은 ICH (International Conference on Harmonisation) 가이드라인에 기술된 선택성, 직선성, 정량한계, 검출한계, 정확성 및 정밀성을 측정하여 분석법의 타당성을 검증하였다. 또한 검증한 분석방법을 이용하여 꾸지뽕나무 열매의 채취시기별 함량을 조사하였다. 그 결과, 미숙과는 7월과 8월에 각 성분의 함량이 증가하였다가 9월에는 감소하였고, 성숙과의 경우 9월 미숙과 보다 각 성분들이 전반적으로 많이 함유되어 있었다.

• Nutrition Research and Practice
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• 제12권1호
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• pp.29-40
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• 2018

BACKGROUND/OBJECTIVES: Ultraviolet radiation (UV) is a major cause of skin photoaging. Previous studies reported that ethanol extract (PET) of Prunus persica (L.) Batsch flowers (PPF, peach flowers) and its subfractions, particularly the ethylacetate (PEA) and n-butanol extracts (PBT), have potent antioxidant activity and attenuate the UV-induced matrix metalloproteinase (MMP) expression in human skin cells. In this study, we investigated the protective activity of PPF extract against UV-induced photoaging in a mouse model. MATERIALS/METHODS: Hairless mice were treated with PET or a mixture of PEA and PBT either topically or orally along with UV irradiation. Histological changes and biochemical alterations of mouse skin were examined. Major phenolic compounds in PPF extract were analyzed using an ACQUITY UPLC system. RESULTS: The overall effects of topical and oral treatments with PPF extract on the UV-induced skin responses exhibited similar patterns. In both experiments, the mixture of PEA and PBT significantly inhibited the UV-induced skin and epidermal thickening, while PET inhibited only the UV-induced epidermal thickening. Treatment of PET or the mixture of PEA and PBT significantly inhibited the UV-induced MMP-13 expression, but not type I collagen expression. Topical treatment of the mixture of PEA and PBT with UV irradiation significantly elevated catalase, superoxide dismutase (SOD) and glutathione-peroxidase (GPx) activities in the skin compared to those in the UV irradiated control group, while oral treatment of the mixture of PEA and PBT or PET elevated only catalase and SOD activities, but not GPx. Thirteen phytochemical compounds including 4-O-caffeoylquinic acid, cimicifugic acid E and B, quercetin-3-O-rhamnoside and kaempferol glycoside derivatives were identified in the PPF extract. CONCLUSIONS: These results demonstrate that treatment with PET or the mixture of PEA and PBT, both topically or orally, attenuates UV-induced photoaging via the cooperative interactions of phenolic components having anti-oxidative and collagen-protective activities.

• Journal of Applied Biological Chemistry
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• 제62권1호
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• pp.31-38
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• 2019

Scutellaria baicalensis Georgi (Scutellariae Radix)는 이뇨제, 고지혈증, 항박테리아, 항알레르기, 항염증제 및 항암제와 같은 건강보조식 및 전통 생약으로도 널리 사용되어 왔다. 본 연구에서 복잡한 S. baicalensis 추출물에서 지표 물질 또는 유효화합물들을 분리하는 것은 신원 확인 및 생리활성 평가를 위한 필수적인 단계다. 8개의 성분들로 구성된 타겟 분획물을 두개의 gradient elution를 사용하여 고성능 액체 크로마토 그래피에서 분석하였다. 중압 액체크로마토그래피 및 개방형칼럼으로 분취를 시뮬레이션함으로 예비실험에서 충분히 분리가 되도록 용리 조건을 결정할 수 있었다. 최적 분취방법으로 확보된 표준유효분획물로부터 8개의 지표성분들이 포함된 것을 확인하였다. 또한, 분획물은 UPLC-QTof-MS 비교 분석으로 MS, UV, HRESIMS 결과를 확인할 수 있었다. 따라서, 스케일 업 실험법은 S. baicalensis 추출물에 성공적으로 적용될 수 있었다.

• 식품기술
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• 제21권2호
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• pp.49-54
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• 2008

농산물 중 잔류농약을 보다 쉽고 효율적으로 분석 할 수 있는 다성분 동시분석 방법에 따라서 UPLC-PDA을 이용하여 기기조건에 따른 검출한계 및 정량한계를 식품별 최저 MRL과 비교하여 유효성을 알아보고 회수율을 통하여 방법의 재현성을 조사한 결과 다음과 같다. 41종의 농약에 대한 검량선은 직선성이 우수하였으며 검출한계 $0.005{\sim}0.109mg/kg$으로 나타났으며 정량한계 는 $0.018{\sim}0.363ppm$으로 나타났다. Cycloprothrin 등의 경우처럼 검출기의 감응도가 최저 MRL 기준을 초과하는 농약에 대한 보완으로는 검출감도가보다 우수한 UV 검출기 등의 병행 활용이 필요하다. 회수율에 따른 재현성은 쌀의 경우 첨가 농도 0.4 mg/kg 일때 $62.09{\sim}99.58%$로 편차범위는 $1.03{\sim}13.92%$ 얻을 수 있었다.

• 분석과학
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• 제27권5호
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• pp.243-247
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• 2014

포름알데히드는 대표적인 직업성 발암물질로, 고농도에 노출되면 사람에게 백혈병이나 임파종, 비인두암 등을 일으킬 수 있다. 본 연구는 포름알데히드의 직업적 노출이 높은 가구목제 제조업 중 1 개 사업장을 대상으로 공정별 공기 중 포름알데히드 농도를 평가하고, 공기 중 포름알데히드 농도가 가장 높은 무늬목 부착 공정에서 사용되는 재료의 실험실내 포름알데히드 발생 및 분석을 통하여 가구 제조 사업장의 포름알데히드의 발생 현황을 파악하고자 하였다. 2,4-디니트로페닐히드라진 코팅 실리카겔 흡착관에 0.2 L/min의 유량으로 6 시간동안 공기 시료를 포집하고 아세토니트릴로 탈착하여 HPLC-UV로 분석하였다. UV 검출 파장은 360 nm였고, ACQUITY UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$, Waters, U.S.A.) 컬럼과 45% 아세토니트릴 이동상을 사용하여 유속을 0.5 mL/min으로 설정하여 분석하였다. 가구 제조 사업장의 포름알데히드 최고 농도는 0.31 ppm으로, 미국 ACGIH의 천장값 농도 기준인 0.3 ppm을 초과하였다. 재단, 조립, 샌딩 등의 공정에서도 포름알데히드 농도는 공장 외부의 농도보다 7-21 배 높은 수준이었다. 무늬목 부착 공정에서 목재로부터 발생하는 포름알데히드는 사업장 실제 적용 온도인 $100-150^{\circ}C$에서 1.14-2.70 ppm으로, 국내 노출기준인 0.5 ppm에 비해 2-5 배 이상 높아, 습식 무늬목을 취급하는 사업장 및 공정 근로자는 포름알데히드에 노출될 가능성이 높은 노출 위험군임을 확인하였다.

• 한국응용과학기술학회지
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• 제29권2호
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• pp.248-256
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• 2012

Aza-indoles are important pharmacophores that have similar size and biological properties of indole. Here we have synthesized 4- and 7-azaindole tryptamines and showed that they are successfully incorporated in the biosynthesis of monoterepene indole alkaloids (MIAs) to form novel azaindole alkaloids by enzymatic reactions of strictosidine synthase(STR) and strictosidine glucosidase(SDG) monitored by UPLC/MS. By using HPLC equipped with a HPLC photo diode array(PDA) detector, each of the UV spectra of azaindole alkaloids was obtained and characterized. When hydrophilicity of azaindole alkaloids was compared, 4-azaindole alkaloids were more hydrophilic than 7-azaindole alkaloids.

• 대한본초학회지
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• 제26권2호
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• pp.11-15
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• 2011

Objectives : In the present study, the contents of cinnamic acid and cinnamaldehyde in three different parts of Cinnamomi Ramulus (CR) (the whole body, the bark part, and the wood part) was evaluated using UPLC (ultra performance liquid chromatography) in order to investigate a suitable cutting method. Methods : Analysis was performed on SMART LC with UV detector. Reference compounds were separated on Inertsil ODS-4 column ($2.1mm{\times}50mm$, $3{\mu}m$, GL Science, Japan) using isolation elution with water and acetonitrile each containing acetic acid at a flow rate of $500{\mu}L/min$. Additionally, samples of CR were purchased from pharmacy of medicinal herb. Results : The correlation coefficients of the cinnamic acid and cinnamaldehyde levels showed good linearity ($r^2{\geq}0.9999$) over the linear ranges. Furthermore, the bark part exhibited higher concentration levels of reference compounds than the wood part in all samples. In addition the bark exfoliation rates in oblique and perpendicular-long cut samples of CR were lower than the perpendicular-short cut samples. Conclusions : These results suggested that the optimal cutting method would be able to reduce the bark exfoliation. Therefore, the oblique or perpendicular-long cutting method is considered to be a better cutting type than the perpendicular-short cutting method.