• Title/Summary/Keyword: HPLC/ELSD

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Determination of Unimark 1494DB in Petroleum using HPLC (HPLC를 이용한 석유제품 중의 식별제 Unimark 1494DB 분석)

  • Lim, Young-Kwan;Kim, DongKil;Yim, Eui Soon;Shin, Seong-Cheol
    • Korean Chemical Engineering Research
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    • v.47 no.5
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    • pp.593-598
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    • 2009
  • In this study, the qualitative and quantitative analytical method for petroleum marker(Unimark 1494DB) in common diesel involved kerosene and byproduct fuel was developed using SPE pretreatment and high performance liquid chromatography. In SPE pretreatment process, the highest concentrated marker was obtained 15 minutes after addition of petroleum sample. The petroleum marker was detected with $1626.92mV{\cdot}sec$ intensity at 9.8 minutes retention time in 1 mg/L content in petrodiesel after pretreatment. Also petroleum marker was selectively identified in an acidic petroleum product which was previously difficult to be analyzed by UV-Vis Spectroscopy.

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.

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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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
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    • v.14 no.4
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    • pp.274-280
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    • 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.
    • 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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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.

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

  • Yoo, Dae-Seok;Choi, Yeon-Hee;Cha, Mi-Ran;Choi, Chun-Whan;Kim, Mi-Ri;Yon, Gyu-Hwan;Hong, Kyung-Sik;Lee, Byung-Hoe;Kim, Eun-Ju;Cho, Sang-Wook;Kim, Young-Sup;Ryu, Shi-Yong;Kang, Jong-Seong
    • Korean Journal of Pharmacognosy
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    • v.41 no.2
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    • pp.147-152
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    • 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.

HPLC Analysis of Saponins in Platycodi Radix (HPLC를 이용한 길경(桔梗) 사포닌 분석법(分析法))

  • Kim, Hyun-Ki;Choi, Jae-Seok;Yoo, Dae-Seok;Choi, Yeon-Hee;Yon, Gyu-Hwan;Hong, Kyung-Sik;Lee, Byung-Hoi;Kim, Hye-Jin;Kim, Eun-Ju;Park, Byoung-Keun;Jeong, Young-Chul;Kim, Young-Sup;Ryu, Shi-Yong
    • Korean Journal of Pharmacognosy
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    • v.38 no.2 s.149
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    • pp.192-196
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    • 2007
  • A rapid and practical HPLC assay was developed for quantitative analysis of saponins in Platycodi Radix. Seven saponin components in Platycodi Radix, i.e., deapioplatycoside E, platycoside E, deapioplatycodin D$_3$, platycodin D$_3$, polygalacin D$_2$, platycodin D$_2$ and platycodin D were successfully resolved on C18 column and detected by ELSD. Standard curves were linear over the concentration range 1 ${\sim}$2,000 ${\mu}$g/ml (r$^2$>0.992). Intra- and inter-day coefficients for variation of seven saponin components were < 10% and limit of quantification of them were around 0.7${\sim}$1.5 ${\mu}$g/ml, respectively. Using this method, contents of seven saponins in various plant materials under different cultivating conditions were estimated.

HPLC/MS/MS Method for Determination of Soyasaponins in the Soybean Varieties (콩 함유 사포닌의 종류 및 함량 분석)

  • Han, Sang-Jun
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.56 no.3
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    • pp.244-249
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    • 2011
  • A sensitive and rapid high-performance liquid chromatographic-tandem mass spectrometric (HPLC/MS/MS) assay was developed for the determination of soyasaponins in soybean. Among soyasaponins, soyasaponin I was isolated and characterized from methanol extracts of soybean as analytical standards and the development of a new analytical procedure for quantification of its content in various cultivars. The structures of these compound was elucidated by $^1H$, $^{13}C$ NMR experiments and by mass spectrometric analysis. Aqueous ethanol extracts of soybean samples were injected on an Agilent XDB-C18 column ($4.6mm{\times}50mm$, $1.8{\mu}m$) with a mobile phase consisting of 10 mM ammonium acetate-acetonitrile, a flow rate of 0.3 mL/min and a total run time of 8 min. Detection was performed by mass spectrometer bin the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI) m/z at 941 ${\rightarrow}$ 615 for soyasaponin I. In the 9 soybean samples, contents of soyasaponin I ranged from 205 to 726 mg/kg, and correlated negatively with seed size.

Saponin Analysis and Red Ginseng Production using the Simplified Method of Korean Ginseng (Panax ginseng C.A.Meyer) (고려인삼(Panax ginseng C.A.Meyer)의 간이법에 의한 홍삼제조 및 사포닌 성분분석)

  • In Jun-Gyo;Kim Eun-Jeong;Lee Bum-Soo;Park Myung-Han;Yang Deok-Chun
    • Korean Journal of Plant Resources
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    • v.19 no.1
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    • pp.133-138
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    • 2006
  • In order to enhance the components of bioactive ginsenosides and the manufacturing process of red ginseng, we developed the simplified method for red ginseng production. The red ginseng extract was prepared from red ginseng produced with the simplified method, and the production rate of extract ($62^{\circ}$ brix) was more than 60%. The ginsenosides of red ginseng were purified and analyzed by HPLC using ELSD. Ginsenoside-$Rg_3,\;Rh_2$ and $Rh_1$, specific artifacts found only in red ginseng, were detected by HPLC. Especially, contents of ginsenoside-$Rg_3$ and Rh1 were detected high than two times in red ginseng produced the simplified method compared to commercial products.