• Title/Summary/Keyword: HPLC-ELSD detector

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

  • Lee, Yong-Hwa;Yang, Jae-Chan;Kim, Chi-Kwang;Lee, Yong-Sub
    • Journal of the Korean Applied Science and Technology
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    • v.32 no.3
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    • pp.461-468
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    • 2015
  • Simultanious quantitative determination of Cetyltrimetyl ammonium chloride(CTM), Stearamidopropyl dimetylamine(SAP), Behentriammonium chloride(BHT), Dihexadeyldimethyl ammonium chloride(DHDDM) was carried out by reversed phase HPLC. The 0.2% TFA/Methanol was used for the mobile phase of gradient conditions. An Alltech $C_{18}$($250mm{\times}4.6mm$ i.d., $5{\mu}m$)and the selected ELSD detector was applied. The analysis results of HPLC showed good linearity with correlation coefficient of $r^2=0.997$ in the rage of $130{\sim}1980.5{\mu}g/mL$ and detection limit.

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.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.238-252
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    • 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.

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Establishment of Analytical Method for Propylene Glycol Alginate in Food Products by Size-exclusion Chromatography (Size-exclusion chromatography법에 의한 식품 중 알긴산프로필렌글리콜 분석법 확립)

  • Jeong, Eun-Jeong;Choi, Yoo-Jeong;Lee, Gunyoung;Yun, Sang Soon;Lim, Ho Soo;Kim, Yong-Suk
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.404-410
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    • 2017
  • An analytical method for determination of propylene glycol alginate (PGA) in food products was developed by HPLC-size-exclusion chromatography. The GF-7M HQ column and LT-ELSD detector were determined by considering the instrumental analysis conditions for PGA analysis. The pretreatment method for the analysis of PGA was suitable for 3 hr extraction at $20^{\circ}C$ and 150 rpm according to the extraction temperature. Linearity ($R^2$) for the analysis of PGA was 0.9873 at calibration curve range of 300, 500, 700, 1,000, and 1,500 mg/kg (5 points). The limit of detection and limit of quantification of PGA on HPLC system was 171.43 and 519.50 mg/kg, respectively. The accuracy and coefficient of variation obtained by size-exclusion chromatography were 86.1~110.4% and 4.1~13.5%, respectively. By applying the HPLC-size-exclusion chromatography system, it was possible to analyze the contents of PGA in 134 different types of food products.

Isolation and Characterization of Major Glycosphingolipid from Rice Bran Extract (쌀겨 추출물로부터 스핑고당지질의 분리와 구조결정)

  • Mitsutake, Susumu;Okada, Tadashi;Kang, Byoung-Won
    • Applied Biological Chemistry
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    • v.50 no.1
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    • pp.72-76
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    • 2007
  • In order to examine the biofunctions of glycosylceramide which is representative of sphingolipid, monoglycosylceramide (cerebroside) was isolated from rice bran extract. Crude glycosylceramides were isolated in large quantities and promptly by flash system column chromatography from rice bran extract, and purified by normal-phase HPLC using an evaporative light-scattering detector. One major cerebroside was obtained by HPLC used as an eluent consisting of chloroform, methanol and water (99:11:1, v/v/v), and the constituents were analyzed by MALDI/TOF-MS, FAB-MS, GC and 600 MHz $^1$H-NMR. The component sugar was estimated to be glucose. In the ceramide, the fatty acid component consist was 2-hydroxy arachidic acid. The long-chain base component was sphinga-4,8-dienine.

The Difference of Ginsenoside Compositions According to the Conditions of Extraction and Fractionation of Crude Ginseng Saponins (추출 및 분획조건에 따른 인삼 조사포닌 중 ginsenoside 조성 차이)

  • Shin, Ji-Young;Choi, Eon-Ho;Wee, Jae-Joon
    • Korean Journal of Food Science and Technology
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    • v.33 no.3
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    • pp.282-287
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    • 2001
  • This study was carried out to investigate the difference of ginsenoside compositions in crude ginseng saponins prepared by five different methods including three new methods. Two known methods are hot methanol(MeOH) extraction/n-butanol(n-BuOH) fractionation and hot MeOH extraction/Diaion HP-20 adsorption/MeOH elution. Three new methods are hot MeOH extraction/cation AG 50W $absorption/H_2O$ elution/n-BuOH extraction, cool MeOH extraction/Diaion HP-20 adsorption/MeOH elution and direct extraction with ethyl acetate(EtOAc)/n-BuOH. Analysis of ginsenoside composition in the crude saponins by conventional HPLC/RI(Refractive Index) did not show great difference between methods except EtOAc/n-BuOH method. However, HPLC/ELSD (evaporative light scattering detector) employing gradient mobile phase afforded fine resolution of ginsenoside Rf, $Rg_1$ and $Rh_1$, and great difference of ginsenoside compositions between methods. LC/MS revealed that large amount of prosapogenins were produced during the pass through the cation exchange (AG 50W) column being strongly acidic. Six major ginsenosides such as $Rb_1,w;Rb_2,$ Rc, Rd, Re and $Rg_1$, 5 prosapogenins and one chikusetsusaponin were identified by LC/MS. A newly established HPLC method employing ODS column and gradient mobile phase of $KH_2PO_4/CH_3CN$ revealed that malonyl ginsenosides were detected only in the crude saponin obtained from cool MeOH extraction.

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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
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    • v.64 no.1
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    • pp.57-61
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    • 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.

Phospholipids Isolation from Squid Viscera Residues After Supercritical Carbon Dioxide Extraction (오징어 내장의 초임계 이산화탄소 추출 잔류물로부터 인지질의 분리)

  • U, Pyoung-Ook;Chun, Byung-Soo
    • Korean Chemical Engineering Research
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    • v.48 no.6
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    • pp.741-746
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    • 2010
  • Phospholipids were recovered from squid viscera residues by ethanol extraction after supercritical carbon dioxide($SCO_2$) extraction and from squid viscera was not processed $SCO_2$ by various organic solvent extraction. $SCO_2$ extraction were performed at $45^{\circ}C$ and 20 MPa for removal of non polar lipid molecules from freeze dried squid viscera sample. Phospholipids were extracted from freeze dried squid viscera sample by chloroform, hexane, methanol, and ethanol and from $SCO_2$extracted squid viscera sample by ethanol. The pH was fixed at 5.7 for all phospholipids extraction conditions. Phospholipid classes were analyzed by HPLC equipped with evaporative light scattering detector (ELSD). Phosphatidyl choline(PC) extracted by ethanol from $SCO_2$ extracted residues was higher than that of extracted by ethanol from squid viscera. But phosphatidyl ethanolamine(PE) and phosphatidic acid(PA) were extracted higher percentage in raw squid viscera. The fatty acid compositions in phospholipids extract by ethanol extract from $SCO_2$ extracted residues were analyzed by gas chromatography(GC). Docosahexanoic acid(DHA) was found in highest percentage in phospholipid extract.

Determination of Fructooligosaccharides and Raffinose in Infant Formula by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSC를 이용한 조제분유 중 fructooligosaccharides 및 raffinose 분석)

  • Shin, Man-Sub;Park, Jae-Woo;Cho, Mi-Ran;Song, Sung-Ok;Kim, Chun-Sun;Choi, Chun-Bae;Lee, Seoung-Won;Lee, Ki-Woong;Chang, Chi-Hoon;Kwak, Byung-Man
    • Korean Journal of Food Science and Technology
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    • v.38 no.6
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    • pp.725-729
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    • 2006
  • A method was developed for the determination of fructooligosaccharides and raffinose contents in infant formula. The samples were extracted and analyzed by liquid chromatography equipped with carbohydrate column and evaporative light scattering detector. The mobile phase used for the gradient mode was water-acetonitrile, at a flow rate of 1.0mL/min. The method showed a mean recovery of 95-99%, the relative standard deviation obtained in the precision study was 0.774-8.982%, the quantification and detection limits were 25-50mg/L.

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

  • Cho, Eun-Jin;Lee, Jong-Ho;Lee, Ki-Teak
    • Korean Journal of Food Science and Technology
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    • v.36 no.4
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    • pp.531-536
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    • 2004
  • Synthesis conditions were optimized using response surface methodology for producing structured lipids (SL) by interesterification of DHA-enriched algae oil derived from microalgae, Schizochytrium sp. and corn oil. Reaction was performed fer 24 hr at $55^{\circ}C$ catalyzed by immobilized lipase from Rhizomucor miehei (RM IM) in shaking water bath. Major fatty acids of SL were palmitic (21.70 mol%), oleic (20.20 mol%), and linoleic (27.34 mol%) acids, and DHA (15.06 mol%). To separate newly synthesized SL-triglycerides (TG) species, HPLC with evaporative light scatting detector (ELSD) was used. Production conditions were optimized using central composite design with reaction temperature $(35-75^{\circ}C,\;X_1)$, reaction time $(2-42\;hr,\;X_2)$, and enzyme concentration $(2-14%,\;X_3)$ as variables. When variables were $70.28^{\circ}C\;(X_1),\;28.74\;hr\;(X_2),\;and\;11.30%\;(X_3)$, maximum content of selected three peaks of synthesized SL-TG species was predicted as 6.97 area%.

Enzymatic synthesis of asymmetric structured lipids containing 1,2-disaturated-3-unsaturated glycerol using acyl migration (효소적 Acyl migration을 이용한 비대칭형 재구성지질(1,2-disaturated-3-unsaturated glycerol)의 합성 및 분석)

  • Hyeon, Jin-Woo;Lee, Ki-Teak
    • Korean Journal of Agricultural Science
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    • v.40 no.4
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    • pp.367-375
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    • 2013
  • The enzymatic interesterification was performed to produce structured lipids (SLs) with palm mid fraction (PMF) and stearic ethyl ester (STEE) for 1, 3, 6, 9, 12 and 15 hr at $80^{\circ}C$. The reaction was catalyzed by Lipozyme TLIM (immobilized lipase from Thermomyces lanuginosus, amount of 20% by weight of total substrates) in a shaking water bath set at 180 rpm. The optimum condition for synthesis of asymmetric SLs were: substrate molar ratio 1:0.5 (PMF:STEE, by weight), reaction time 6 hr, enzyme 20% (wt%, water activity=0.085) of total substrate and reaction temperature $80^{\circ}C$. After reaction at optimized condition, triacylglycerols (symmetrical and asymmetrical TAGs) from reactants were isolated. POP/PPO (1,3-palmitoyl-2-oleoyl glycerol or 1,2-palmitoyl-3-oleoyl glycerol), POS/PSO (palmitoyl-oleoyl-stearoyl glycerol or palmitoyl-stearoyl-oleoyl glycerol), SOS/SSO (1,3-stearoyl-2-oleoyl glycerol or 1,2-stearoyl-3-oleoyl glycerol) were obtained by solvent fractionation. Finally, refined SLs contained stearic acid of 16.91%. Solid fat index and thermogram of the refined SLs were obtained using differential scanning calorimetry. The degree of asymmetric triacylglycerol in the refined SLs was analyzed by Ag-HPLC equipped with evaporated light scattering detector (ELSD). The refined SLs consisted of symmetric TAG of 41.15 area% and asymmetric TAG of 58.85 area%.