• Title/Summary/Keyword: HPLC quantification

검색결과 403건 처리시간 0.022초

건강기능식품 등 중 수용성 비타민 B군의 HPLC를 이용한 동시분석법 (Simultaneous Determination of Water Soluble Vitamins B Group in Health Functional Foods etc. by HPLC)

  • 김선희;김재현;이화정;오재명;이성혜;반경녀;서일원;이영주;이진희;강태석
    • 한국식품위생안전성학회지
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    • 제30권2호
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    • pp.143-149
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    • 2015
  • 건강기능식품 등 중 수용성 비타민 B군 (비타민 $B_1$, 비타민 $B_2$, 나이아신, 비타민 $B_6$)의 동시분석 방법을 확립하기 위하여 본 연구를 실시하였다. HPLC에 의한 수용성 비타민 B군의 분석 방법은 기기분석조건을 확립하고, 국내외 시험법 및 논문을 참고하여 시험 데이터를 분석하였다. 수용성 비타민 B군의 HPLC 분석은 270 nm에서 Capcell Pak C18 UG 120 컬럼을 사용하여 진행되었다. 분석법 검증은 수용성 비타민 B군의 직선성, 정확성, 정량한계, 정밀성에 대해 수행되었다. 직선성은 비타민 $B_1$, 비타민 $B_2$, 나이아신(nicotinic acid, nicotinamide), 비타민 $B_6$ 모두 $0.1{\sim}2{\mu}m/mL$의 농도범위에서 $R^2=0.999$ 이상의 우수한 직선성을 확인할 수 있었다. 회수율을 검토한 결과, 비타민 $B_1$ 100~103%, 비타민 $B_2$ 104~112%, nicotinic acid 82~85%, nicotinamide 121~124%, 비타민 $B_6$ 95~104%의 양호한 회수율을 확인할 수 있었다. LOQ는 비타민 $B_1$ $0.04{\mu}m/mL$, 비타민 $B_2$ $0.05{\mu}m/mL$, nicotinic acid $0.15{\mu}m/mL$, nicotinamide $0.08{\mu}m/mL$, 비타민 $B_6$ $0.63{\mu}m/mL$ 이었다. 정밀성을 검토한 결과, $B_1$ 0.4%, 비타민 $B_2$ 0.4%, nicotinic acid 0.5%, nicotinamide 0.7%, 비타민 $B_6$ 0.4%로 1% 이내로 양호한 재현성을 확인할 수 있었다. 또한 동시분석법의 정확성을 검증하기 위하여 어린이 기호식품 및 건강기능식품의 표시함량 모니터링을 수행한 결과, 모두 표시기준에 적합함을 확인할 수 있었다.

섬쑥부쟁이 에탄올 추출물의 잔틴산화효소 저해 효능 및 HPLC-UV를 이용한 유효성분의 함량 분석 (Inhibitory Effects of Ethanolic Extracts from Aster glehni on Xanthine Oxidase and Content Determination of Bioactive Components Using HPLC-UV)

  • 강동현;한은혜;진창배;김형자
    • 한국식품영양과학회지
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    • 제45권11호
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    • pp.1610-1616
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    • 2016
  • 섬쑥부쟁이로부터 고요산혈증 개선에 도움을 주는 기능성 식품 개발을 위하여 최적의 에탄올 추출물 탐색과 high performance liquid chromatography-ultraviolet(HPLC-UV) 분석방법에 의한 validation을 실시하였다. 지표성분으로 3,5-dicaffeoylquinic acid(3,5-DCQA)를 선정하여 표준화를 실시하였으며 검출법 확립을 위한 3,5-DCQA 정량분석은 Luna RP-18 칼럼($4.6{\times}250mm$, $5{\mu}m$)을 이용하여 1% 초산용액과 메탄올을 전개용매로 사용하였다. 용출은 1.0 mL/min의 유속으로 기울기 용출(gradient elution) 방법을 이용하였으며, 320 nm 파장에서 검출한 피크 면적을 이용하여 검량곡선을 작성하여 분석하였다. 본 연구에서 확립한 분석법으로 특이성, 직선성, 정밀성, 정확성, 회수율을 검색하였다. 3,5-DCQA의 검량선으로부터 상관계수($R^2$) 0.9999의 우수한 직선성과 intra-day와 inter-day 분석에서 90% 이상의 회수율과 5% 미만의 RSD를 나타내 정밀성과 정확성을 입증하였다. 검출한계는 $2.68{\mu}g/mL$였고 정량한계는 $8.11{\mu}g/mL$로 나타났다. 섬쑥부쟁이 에탄올 추출물(AGE)은 70과 $80^{\circ}C$에서 30, 50, 70, 80% 에탄올로 3, 4, 5, 6시간 동안 각각 추출하였으며, 지표물질의 검량곡선을 활용하여 각각의 AGE로부터 3,5-DCQA의 함량을 분석하였다. 본 시험법으로 분석한 3,5-DCQA의 함량은 $70^{\circ}C$에서 추출한 70% AGE가 $52.59{\pm}3.45mg/Aster$ glehni 100g의 함량을 나타내 가장 우수하게 나타났다. 그러나 섬쑥부쟁이 추출물에 함유된 5-caffeoylquinic acid(5-CQA)의 함량 비교분석은 에탄올 함량이나 추출 시간에 따른 함량 변화가 미미하게 나타났다. 또한, 다양한 AGE에 대하여 XOD 저해 효능을 검색하였을 때, 3,5-DCQA의 함량이 가장 높은 $70^{\circ}C$에서 추출한 70% AGE에서 우수한 효능을 나타내 기능성 원료 표준화를 위한 적합한 분석법임이 검증되었다. 따라서 본 연구를 통하여 확립된 3,5-DCQA의 분석법은 섬쑥부쟁이 에탄올 추출물로부터 개별인정형 건강기능식품 기능성 원료 개발을 위한 유용한 자료로 활용될 것으로 생각한다.

Determination of Ginsenosides Content in Korean Ginseng Seeds and Roots by High Performance Liquid Chromatography

  • Hu, Jiang Ning;Lee, Jeung-Hee;Shin, Jung-Ah;Choi, Jae-Eul;Lee, Ki-Teak
    • Food Science and Biotechnology
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    • 제17권2호
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    • pp.430-433
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    • 2008
  • A high performance liquid chromatography (HPLC) method has been successfully developed to identify and quantify major ginsenosides in Korean ginseng seeds and roots. Using gradient elution of acetonitrile and water without buffer, the 6 major ginsenosides ($Rb_1,\;Rb_2$, Rc, Rd, Re, and $Rg_1$) were identified. Compared with ginseng roots, the amount of ginsenoside Re and Rd in ginseng seeds were significantly higher than those in ginseng roots (p<0.05). In ginseng seeds, the content of protopanaxtriol (PPT) was higher than that of protopanaxdiol (PPD) and the ratio of PPT and PPD was approximately 2.2 : 1. However, the content of PPT was lower than that of PPD in ginseng roots. It should be mentioned that both content of PPT and PPD in ginseng seeds were much higher than those in ginseng roots.

Bioconversion of Acrylonitrile to Acrylic Acid by Rhodococcus ruber Strain AKSH-84

  • Kamal, Ahmed;Kumar, M. Shiva;Kumar, C. Ganesh;Shaik, Thokhir Basha
    • Journal of Microbiology and Biotechnology
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    • 제21권1호
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    • pp.37-42
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    • 2011
  • A new versatile acrylonitrile-bioconverting strain isolated from a petroleum-contaminated sludge sample and identified as Rhodococcus ruber AKSH-84 was used for optimization of medium and biotransformation conditions for nitrilase activity to produce acrylic acid. A simple and rapid HPLC protocol was optimized for quantification of acrylic acid, acrylamide, and acrylonitrile. The optimal medium conditions for nitrilase activity were pH of 7.0, temperature of $30^{\circ}C$, agitation of 150 rpm, and inoculum level of 2%. Glycerol as a carbon source and sodium nitrate as the nitrogen source provided good nutritional sources for achieving good biotransformation. Nitrilase activity was constitutive in nature and was in the exponential growth phase after 24 h of incubation under optimal conditions without addition of any inducer. The substrate preference was acrylonitrile and acetonitrile. The present work demonstrates the biotransformation of acrylonitrile to acrylic acid with the new strain, R. ruber AKSH-84, which can be used in green biosynthesis of acrylic acid for biotechnological processes. The nitrilase produced by the isolate was purified and characterized.

Simplified HPLC Method for the Determination of Prazosin in Human Plasma and Its Application to Single-dose Pharmacokinetics

  • Gwak, Hye-Sun;Chun, In-Koo
    • Biomolecules & Therapeutics
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    • 제13권2호
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    • pp.90-94
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    • 2005
  • Prazosin hydrochloride is an antihypertensive drug with selective ${\alpha}_1$-adrenoreceptor blocking effects. A simple high performance liquid chromatographic method has been developed and validated for the quantitative determination of prazosin in human plasma. A reversed-phase C18 column was used for the separation of prazosin and terazosin (internal standard) with a mobile phase composed of water, acetonitrile and triethylamine(75:25:0.1, V/V;pH5.0) at a flow rate of 1.5 ml/min. the fluorescence detector was set at excitation and emissionwavelengths of 250 and 370 nm, respectively. Intra-and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification of 0.5 ng/ml. Good recovery (>80%) was seen in plasma. Prazosin was stable in human plasma under various storage conditions. This method was used successfully for a pharmacokinetic study in plasma after oral administration of a single 2-mg dose as prazosin base to 16 healthy volunteers. The maximum plasma concentration of prazosin was 23.1 ${\pm}$ 16.5 ng/ml at 2.1 h, and the mean area under the curve and elimination half-life were calculated to be 108.4 ${\pm}$ 74.2 ng ${\cdot}$hr/ml and 2.5 ${\pm}$ 0.6 h, respectively.

EBM 기반구축을 위한 평위산 전임상 연구 문헌 분석 (Analysis of Studies on Pyeongwi-san to Establish the Fundament for Evidence Based Medicine)

  • 김정훈;이준경;신현규
    • 동의생리병리학회지
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    • 제24권5호
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    • pp.770-778
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    • 2010
  • To establish the fundament for EBM of Traditional Korean Medicine, the papers on Pyeongwi-san (Pingwei-san) frequently used in medical institutions of Traditional Korean Medicine were analyzed through researching domestic and international papers. The papers were classified by the registration of domestic or international journals, the year of publishment, experimental fields and the kinds of studies on biological activities. Of total 518 papers on Pyeongwi-san (Pingwei-san), 32 volumes were selected according to selection creteria. 20 volumes were published in domestic journals, 11 in Chinese journal and 1 in Japanese journal. The papers on instrumental analyses reported the quantification of standard compounds of herbal medicines in Pyeongwi-san (Pingwei-san) using HPLC, GC-MS. The papers on biological activities of Pyeongwi-san (Pingwei-san) showed improvement of gastrointestinal activity and water-electrolyte metabolism, immune regulation, anti-oxidant, anti-inflammatory, analgesic, anti-convulsant activities, hypnotic duration, blood pressure regulation, hepatic protection, congestive heart failure, anti-cancer activities. Further studies including gastrointestinal activity need to be preceeded to establish the fundament for EBM of Pyeongwi-san (Pingwei-san).

HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증 (Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation)

  • 윤형준;윤소미;이명헌;손성완
    • 대한수의학회지
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    • 제48권1호
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    • pp.33-38
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    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).

염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석 (Determination of Polychlorinated Biphenyls in the Soil by Perchlorination)

  • 문철호;최상기;김정호
    • 한국환경과학회지
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    • 제4권3호
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    • pp.97-97
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석 (Determination of Polychlorinated Biphenyls in the Soil by Perchlorination)

  • 문철호;최상기;김정호
    • 한국환경과학회지
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    • 제4권3호
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    • pp.249-258
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

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민박쥐나물 추출물의 Caffeoylquinic Acid 정량 및 Acetylcholinesterase 활성과 Peroxynitrite 농도에 대한 효과 (Quantification of Caffeoylquinic Acids and the Effect of the Cacalia hastata var. orientalis Extract on Acetylcholinesterase Activity and Peroxynitrite Concentration)

  • 누그로호 아궁;최재수;박희준
    • 생약학회지
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    • 제48권3호
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    • pp.243-247
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    • 2017
  • To find the anti-Alzheimer's activity of Cacalia hastata var. orientalis (Compositae), caffeoylquinic acids were analyzed in this plant by HPLC and the inhibitory activities of the extract on cholinesterases including acetylcholinesterase (AChE) and butyrylcholinesterse (BChE) and peroxynitrite ($ONOO^-$) were assayed. Sum of caffeoylquinic acids in the 80% MeOH extract was quantitatively higher in leaves (35.8% of the extract) than in stems (3.7%). The compound, 3,5-dicaffeoylquinic acid, was contained in the highest amount in the leaf (44.32 mg/g dry weight). The $IC_{50}s$ of the 80% MeOH extract were shown to be $67.45{\mu}g/ml$ for AChE, and $8.59{\mu}g/ml$ (for $ONOO^-$), respectively, suggesting that the leaves would have the anti-Alzheimer's activity due to the high content of caffeoylquinic acids.