• 제목/요약/키워드: ELSD

검색결과 60건 처리시간 0.024초

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

  • Yeom, Hye-Sun;Suh, Joon-Hyuk;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
    • /
    • 제31권5호
    • /
    • pp.1159-1164
    • /
    • 2010
  • Several triterpenoid saponins from root of Pulsatilla koreana Nakai (Ranunculaceae) were studied and their biological activities were reported. It is difficult to analyze triterpenoid saponins using HPLC-UV due to the lack of chromophores. So, evaporative light scattering detection (ELSD) is used as a valuable alternative to UV detection. More recently, a charged aerosol detection (CAD) has been developed to improve the sensitivity and reproducibility of ELSD. In this study, we developed and validated a novel method of high performance liquid chromatography coupled with a charged aerosol detector for the simultaneous determination of four triterpenoid saponins: pulsatilloside E, pulsatilla saponin H, anemoside B4 and cussosaponin C. Analytes were separated by the Supelco Ascentis$^{(R)}$ Express C18 column (4.6 mm ${\times}$ 150 mm, 2.7 ${\mu}m$) with gradient elution of methanol and water at a flow rate of 0.8 mL/min at $30^{\circ}C$. We examined various factors that could affect the sensitivity of the detectors, including various concentrations of additives, the pH of the mobile phase, and the CAD range. Linear calibration curves were obtained within the concentration ranges of 2 - 200 ${\mu}g$/mL for pulsatilloside E, anemoside $B_4$ and cussosaponin C, and 5 - 500 ${\mu}g$/mL for pulsatilla saponin H with correlation coefficient ($R^2$) greater than 0.995. The limit of detection (LOD) and quantification (LOQ) were 0.04 - 0.2 and 2 - 5 ${\mu}g$/mL, respectively. The validity of the developed HPLC-CAD method was confirmed by satisfactory values of linearity, intra- and inter-day accuracy and precision. This method could be successfully applied to quality evaluation, quality control and monitoring of Pulsatilla koreana.

역상 HPLC에 의한 Fatty quaternary ammonium salt 4종 동시분석 (Simultaneous determination of Fatty quaternary ammonium salt by RP-HPLC)

  • 이용화;양재찬;김재광;이용섭
    • 한국응용과학기술학회지
    • /
    • 제32권3호
    • /
    • pp.461-468
    • /
    • 2015
  • 역상 HPLC에 의한 Cetyltrimetyl ammonium chloride(CTM), Stearamidopropyl dimetylamine(SAP), Behentriammonium chloride(BHT), Dihexadeyldimethyl ammonium chloride (DHDDM)의 양이온계면활성제 4종 동시 정량분석 방법을 개발하였다. 분석조건으로 분리관은 Alltech $C_{18}$($250mm{\times}4.6mm$ i.d., $5{\mu}m$)을 사용하였고, 검출기는 ELSD를 사용하였으며, 이동상은 0.2% TFA/Methanol의 기울기 용리에 의해 분석되었다. 이때 검량선의 상관계수($r^2$)는 $130{\sim}1980.5{\mu}g/mL$농도 범위에서 0.997이상 이었고, 검출한계, 정밀성이 우수하였다. 이 방법은 fatty quaternary ammonium salt 4종의 정량분석 가능함을 보여 주었다.

Compositional Analysis of Major Saponins and Anti-inflammatory Activitiy of Steam-Processed Platycodi Radix under Pressure

  • Ha, In-Jin;Chung, Ji-Won;Ha, Young-Wan;Shin, Eun-Myoung;Kim, Yeong-Shik
    • Natural Product Sciences
    • /
    • 제14권4호
    • /
    • pp.274-280
    • /
    • 2008
  • Platycosides are the saponins in Platycodi Radix and they have several beneficial effects such as antiinflammatory and anti-obesity activities. This study was designed to determine the changes in the saponin composition in Platycodi Radix (platycosides) after being processed under steam and pressure and to investigate the anti-inflammatory effects of their extracts. The change of the platycoside compositions was investigated after 1, 2, 3, 6 and 9h heat processing of Platycodi Radices by using HPLC coupled with an evaporative light scattering detection (ELSD) system. After heat treatment ($125^{\circ}C$, 1, 2, 3, 6 and 9 h), the contents of several platycosides such as platycoside E, platycodin $D_3$, platycodin D, polygalacin D, and platycodin A decreased as the processing time was longer. While the total contents of the saponins decreased, the contents of deapi-forms of deapiplatycoside E, deapi-platycodin $D_3$, and deapi-platycodin D increased relatively. These results indicate that the linkage between apiose and xylose located at C-28 is labile to heat and pressure. The LPS-induced iNOS inhibitory activities of the samples treated for 1 and 2 hours were enhanced and after then, the activities were reduced. These results suggested that heat treatment of the samples affect the content of the total saponins and the saponin content may be the important criteria representing the anti-inflammatory activity.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • 고려인삼학회:학술대회논문집
    • /
    • 고려인삼학회 2002년도 학술대회지
    • /
    • pp.238-252
    • /
    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

  • PDF

Saccharomyces cerevisiae 의 회분식 배양에서 세라마이드의 생산 (The ceramide contents of Saccharomyces cerevisiae in batch culture)

  • 김세경;노용호;윤현식
    • KSBB Journal
    • /
    • 제23권5호
    • /
    • pp.449-451
    • /
    • 2008
  • Saccharomyces cerevisiae를 배양하여 ceramide를 생산하였다. 각기 다른 growth phase에서의 ceramide 생산량을 비교 실험하였다. Ceramide는 ELSD가 장착된 HPLC를 통하여 분석하였으며 stationary phase에 접어든 후 12시간 후에 회수, 추출된 양(2.01 mg ceramide/g cell)이 최대인 것으로 나타났다.

조류(microalgae)에서 얻어진 DHA powder로부터의 유지 추출 및 특성 연구

  • 조은진;이기택
    • 한국식품저장유통학회:학술대회논문집
    • /
    • 한국식품저장유통학회 2003년도 제23차 추계총회 및 국제학술심포지움
    • /
    • pp.141.2-141
    • /
    • 2003
  • 고도불포화지방산 중 EPA(eicosapentaenoic acid)와 DHA(docosahexaenoic acid)는 여러 가지 생리활성 효과를 나타내는 것으로 알려져 있으며, 최근 관심이 주목되고 있다. 본 실험에서는 특히 DHA의 함량이 높은 해양미생물, 즉 조류(microalgae)인 Schizochytrium sp.에서 얻어진 DHA powder로부터 두 가지 방법으로 유지를 추출한 뒤 그 성질을 비교.분석하였다. 먼저, 8$0^{\circ}C$, soxhlet extractor로부터 6시간 동안 추출하고, 55$^{\circ}C$, shaking water bath로부터 같은 시간 동안 추출한 결과, 각각 25.5, 24.0%의 수율을 나타내었다. GC에 의한 지방산 조성 분석 결과, soxhlet extractor에서 추출한 경우, palmitic acid, DHA가 각각 30.98, 30.04 mol%로 주요 지방산인 것으로 나타났으며, shaking water bath에서 추출된 유지는 그 함량이 각각 31.44, 34.78 mol%를 나타내었다. 또한 pancreatic lipase에 의한 가수분해를 통해 sn-2 위치의 지방산 조성 분석 결과, DHA가 sn-2 위치에 주로 함유되어있는 것으로 조사되었다. 한편, HPLC-ELSD system을 이용하여 중성지방의 구성 성분을 분석 결과, 유지의 99%이상이 TAG(triacylglycerol) 형태로 이루어져 있었으며, 소량의 MAG(monoacylglycerol) 존재를 확인할 수 있었다.

  • PDF

Universal LC Method for a Determination of Fourteen Cationic Surfactants Widely Used in Surfactant Industry

  • Ryu, Ho-Ryul;Park, Hong-Soon;Rhee, Choong-Kyun
    • Bulletin of the Korean Chemical Society
    • /
    • 제28권1호
    • /
    • pp.85-88
    • /
    • 2007
  • Ab initio periodic Hartree-Fock calculations with the full potential and minimum basis set are applied to interpretation of scanning tunneling microscope (STM) and atomic force microscope (AFM) images on 1TVTe2. Our results show that the simulated STM image shows asymmetry while the simulated AFM image shows the circular electron densities at the bright spots without asymmetry of electron density to agree with the experimental AFM image. The bright spots of both the STM and AFM images of VTe2 are associated with the surface Te atoms, while the patterns of bright spots of STM and AFM images are different.

Simultaneous determination of saikosaponin derivatives in Bupleurum falcatum by HPLC-ELSD analysis using different extraction methods

  • Choi, Jungwon;Kim, Juree;Kang, Sam Sik;Lee, Sanghyun
    • Journal of Applied Biological Chemistry
    • /
    • 제64권1호
    • /
    • pp.57-61
    • /
    • 2021
  • Saikosaponin derivatives such as saikosaponins A, B1, B2, B3, B4, C, and D present in Bupleurum falcatum were analyzed by a high performance liquid chromatograph equipped with an evaporative light scattering detector, using different extraction solvents (water and 70% ethanol). The samples were injected into a YMC Pack Pro C18 column and separated using a gradient elution system with a mobile phase composed of acetonitrile and water at a flow rate of 1.1 mL/min. The content of saikosaponin derivatives was higher in 70% ethanol extract than in water extract. This study provides an efficient analytical method for determining the optimal conditions for extraction of saikosaponin derivatives, which can be used as a basis for development of functional foods and pharmaceutical products from B. falcatum.

반응표면분석에 의한 기능성 유지의 효소적 합성 조건 최적화 (Optimization of Enzymatic Synthesis Condition of Structured Lipids by Response Surface Methodology)

  • 조은진;이종호;이기택
    • 한국식품과학회지
    • /
    • 제36권4호
    • /
    • pp.531-536
    • /
    • 2004
  • Omega-3 지방산인 DHA가 풍부하고 이취가 적은 조류(microalgae, Schizochytrum sp.)로부터 지질을 획득하여 이를 옥수수유와 기질로 이용, 고정화효소인 RM IM(from Rhizomucormiehei)을 촉매로 하여 interesterification 반응에 의해 고기능성 유지를 효과적으로 생성하기 위하여 합성조건을 반응표면분석에 의해 최적화하였다. 항온교반수조에서 소량 합성된 재구성 지질의 TG 지방산 조성 분석 결과, 재구성지질에 함유된 DHA의 함량은 15.06mol%를 나타내었고, DHA-enriched algae oil에 과량 함유된 palmitic acid(30.67mo1%), myristic acid(11.64mol%)의 함량은 각각 30, 60% 감소하여 21.70, 4.96 mol%를 보였으며, oleic과 linoleic acid의 함량은 급격히 증가하여 각각 20.20, 27.34 mo1%를 나타내었다. RP HPLC-ELSD system을 이용하여 재구성지질의 TG 형태를 분리한 결과, 두 기질에 존재하지 않은 다수의 새로운 TG peak를 확인한 수 있었으며, 이중 쉽게 식별이 가능한 3개의 peak를 선택, 이들 peak area% 총합을 반응변수로 하고 온도$(35-75^{\circ}C,\;X_1)$, 시간(2-42시간, $X_2$) 및 효소농도(2-14%, $X_3$)를 요인변수로 하여 중심합성계획에 의해 반응조건을 최적화하였다. 그 결과, 온도$(70.28^{\circ}C)$, 시간(28.74시간), 효소농도(11.30%)의 최적합성조건에서 최대값 6.97 area%로 예측되었다.

길경(桔梗)의 추출조건에 따른 사포닌함량의 변화 (제2보) (Variation of Saponin Content in the Decoctions of Platycodi Radix (II))

  • 유대석;최연희;차미란;최춘환;김미리;연규환;홍경식;이병회;김은주;조상욱;김영섭;유시용;강종성
    • 생약학회지
    • /
    • 제41권2호
    • /
    • pp.147-152
    • /
    • 2010
  • The capability of the solvents for extracting the bioactive saponins from the roots of Platycodon grandiflorum (Campanulaceae) was investigated to obtain an ideal extract which contained bioactive saponins with high quality and high quantity. The content of eight representative saponins in extracts, such as deapioplatycoside E, platycoside E, platyconic acid A and platycodin D, platycodin $D_3$, platycodin $D_2$, polygalacin $D_2$, polygalacin D were analyzed simultaneousely by the modified HPLC analytical method. The validation test of the modified qualitative and quantitative analytical method employing the ELSD equipped HPLC for eight representative saponins in the roots extract of P. grandiflorum showed a good linearity, precision and accuracy. the correlation coefficient ($r^2$) values of the calbration curves for each saponins were observed to be over 0.9990. LOD and LOQ of each saponin was calculated as $0.10{\mu}g{\sim}0.40{\mu}g$ (LOD) and $0.40{\mu}g{\sim}0.80{\mu}g$ (LOQ), respectively. Recovery rates of each saponin were also calculated as over 98%, respectively. With exception of two saponins, platyconic acid A and platycodin D, The content of eight saponins in extracts was decreased proportionally to the increment of the water ratio of solvent for extraction. Consequently, as aquous alcohol was used as a solvent for extracting the saponin components from powdered roots of P. grandiflorum, the water content in the aquous alcohol was seemed to be a critical factor for extracting efficacy. The 60-80% ratio of alcohol in the aquous alcohol were deduced to be suitable and recommendable for the preparation of roots extract of P. grandiflorum which contained saponins with high quality and high quantity.