• 제목/요약/키워드: column switching

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Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제34권12호
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

Achiral/Chiral Coupled Column법에 의한 식품 중의 D-아미노산의 정량분석 (Micro-Determination of D-Amino Acids in Food by Using Achirai/Chiral Coupled Column Method)

  • 이선행;장윤희;이광필
    • 분석과학
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    • 제9권1호
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    • pp.52-61
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    • 1996
  • 식품 중의 몇몇 유리 D-아미노산이 column switching method에 의해 검출되었다. D-아미노산과 L-아미노산의 총량의 정량은 $C_{18}$ 컬럼을 사용한 비키랄 분리에 근거한다. L-아미노산에 대한 D-아미노산의 수준은 o-phthalaldehyde로 유도체화된 아미노산의 postcolumn reaction detection을 포함하는 column switching system에 의해 정량되었다. Postcolumn detection system의 키랄 분리는 chiral crown ether 컬럼에 의해 실행되었다. 이 system은 간장과 발효된 콩, 그리고 콩 같은 식품 중에 있는 D-아미노산의 정량에 적용된다. 이 achiral/chiral coupled-column system하에서는 시료 전처리과정이 중요함을 알게 되었다. Phenylalanine은 시판용 간장 속에 242ppm, 재래식 간장 속에는 102ppm, 발효된 콩에는 1g당 8.34mg, 콩에는 1g당 2.87mg이 함유된 것으로 밝혀졌다. D-phenylalanine은 시판용 간장 속에는 0.67%, 재래식 간장에는 0.34%, 발효된 콩에는 1.81% 미만, 콩에는 2.82% 미만이 검출되었다.

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DETERMINATION OF SIMVASTATIN IN HUMAN PLASMA BY COLUMN SWITCHING HPLC WITH UV DETECTION

  • Ban, Eun-Mi;Kim, Bae-Chan;Park, Tae-Hwan;Kim, Chong-Kook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.281.1-281.1
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    • 2003
  • Purpose. The purpose of this study was to develop and validate sensitive and specific analytical method for determinination of simvastatin in human plasma by the column-switching high-performance liquid chromatography (HPLC) system with UV detection. Methods. Simvastatin and internal standard were extracted into diethyl ether from plasma. (omitted)

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Simple and Sensitive Determination of Baclofen in Human Plasma by Column-Switching and Semi-Micro High-Performance Liquid Chromatography

  • Ban, Eun-Mi;Ko, Hye-Ran;Kim, Chong-Kook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.284.2-284.2
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    • 2003
  • Using a column-switching technique. highly sensitive and selective semi-micro high-performance liquid chromatographic (HPLC) method has been developed for the determination of baclofen in human plasma. Following precipitation of plasma sample containing baclofen with zinc sulfate-acetonitrile, samples were directly injected on to the system. (omitted)

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Determination of Phthalate Metabolites in Human Serum and Urine as Biomarkers for Phthalate Exposure Using Column-Switching LC-MS/MS

  • Jeong, Jee-Yeon;Lee, Ji-Hyun;Kim, Eun-Young;Kim, Pan-Gyi;Kho, Young-Lim
    • Safety and Health at Work
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    • 제2권1호
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    • pp.57-64
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    • 2011
  • Objectives: Although phthalates like dibutyl phthalate (DBP) and di-2-ethylhexyl phthalate (DEHP) are commonly used as plasticizers and their metabolites are especially suspected of reproductive toxicity, little is known about occupational exposure to those phthalates. The aim of this study was to assess the utility of measuring the metabolite concentrations of DBP and DEHP in serum and urine samples as an indicator of occupational exposure to those phthalates. Methods: Phthalate metabolites were analyzed by using column-switching high-performance liquid chromatography tandem mass spectrometry (LC-MS/MS). Results: We detected phthalate metabolites in serum and urine matrices at approximately 10-fold lower than the limit of detection of those metabolites in the same matrix by LC-MS/MS without column switching, which was sufficient to evaluate concentrations of phthalate metabolites for industrial workers and the general population. Conclusion: The accuracy and precision of the analytical method indicate that urinary metabolite determination can be a more acceptable biomarker for studying phthalate exposure and adverse health outcomes.

Determination of rebamipide in human plasma by column-switching high- performance liqiud chromatography.

  • Koung, Joung-Sun;Park, Chang-Hun;Kim, Ho-Hyun;Lee, Hee-Joo;Beom, Han-Sang
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.278.2-278.2
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    • 2003
  • A column-switching semi-micro HPLC method with fluorescence detection was developed for the direct analysis of rebamipide in human plasma. Plasma was filtered through a 0.45 $\mu\textrm{m}$ membrane filter and 5 ${\mu}\ell$ of the filtrate was directly injected onto the pre-column. After elution of the plasma proteins to waste, the retained rebamipide and internal standard(ofloxacin) were transferred to a C18 semi-microcolumn (5$\mu\textrm{m}$, 150 ${\times}$2.0mm) where they were separated using acetonitrile-1.4% acetic acid (40:60, v/v) as mobile phase. (omitted)

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컬럼스위칭 액체크로마토그래피를 이용한 뇨중 플루비프로펜의 광학이성질체의 미량분석 (Trace Analysis of Racemic Isomers of Flurbiprofen in Human Urine using Column Switching-HPLC)

  • 최현철;강신정;윤미옥;이수정;김호정;박창훈;차기원
    • 분석과학
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    • 제15권6호
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    • pp.529-533
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    • 2002
  • 광학이성질체 분리 컬럼, 시료처리 및 농축 컬럼이 부착된 컬럼스위칭-HPLC를 이용하여 뇨시료에서 미량의 플루비프로펜 광학이성질체를 분리 정량하는 방법을 연구하였다. 분리된 각 이성질체의 고유광회전도를 구하고, d-이성질체 및 l-이성질체를 확인하였다. 이들의 검정선의 농도범위는 각각 $0.11{\sim}5.4{\mu}g/mL$이었으며, 검출한계는 d-이성질체의 경우 $0.027{\mu}g/mL$이고, l-이성질체의 경우 $0.031{\mu}g/mL$이며, 날자간 및 날자내의 정밀도의 CV값은 각각 1.84% 이하였다. 본 분석법은 플루비프로펜 약물을 복용한 살마의 뇨중에 존재하는 플루비프로펜의 분석에 적용하였다.

Development of Vitamin D Determination in Infant Formula by Column-Switching HPLC with UV Detector

  • Ko, Jin-Hyouk;Kwak, Byung-Man;Ahn, Jang-Hyuk;Shim, Sung-Lye;Kim, Kyong-Su;Yoon, Tae-Hyung;Leem, Dong-Gil;Jeong, Ja-Young
    • 한국축산식품학회지
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    • 제32권5호
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    • pp.571-577
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    • 2012
  • This study was carried out to develop an analytical method for the determination of vitamin D in infant formula. Vitamin D was determined by column-switching high-performance liquid chromatography (HPLC) equipped with a reversed phase column and UV detector after saponification and extraction of the formula with an organic solvent. A preseparation column ($C_8$), focusing column ($C_{18}$), analytical column ($C_{18}$) and UV-Vis detector (254 nm) were used. The limits of detection (LOD) and the limits of quantification (LOQ) for vitamin D were estimated to be $1.51{\mu}g/kg$ and $4.95{\mu}g/kg$, respectively. The linearity, recovery, precision and accuracy of the analytical method for vitamin D were evaluated through the application of a SRM (Standard Reference Material) 1846 (National Institute of Standard & Technology, USA). The linearity of this method was calculated with a value of the coefficient of determination ($r^2$) ${\geq}0.9999$. The recovery of vitamin D was $85.20{\pm}3.00%$. The intra-assay precision for vitamin D was between $1.68{\pm}0.03%$ and $5.75{\pm}0.33%$, and the inter-assay precision for vitamin D ranged from $1.73{\pm}0.03%$ to $2.96{\pm}0.09%$. The intra-assay accuracy for vitamin D was between $100.03{\pm}2.77%$ and $102.01{\pm}0.59%$, and the inter-assay accuracy for vitamin D ranged from $99.00{\pm}1.53%$ to $102.01{\pm}3.04%$. The proposed method is optimal for the separation and quantification of vitamin D from infant formula.

Preparative Chromatographic Separaction: Simulated Moving Bed and Modified Chromatography Methods

  • Yi Xie;Koo, Yoon-Mo;Nien-Hwa Linda Wang
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제6권6호
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    • pp.363-375
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    • 2001
  • Chromatography has been method of choice for the separation complex biologi-cal mixtures fro analytical purpose, particularly for the last fifty years. Its use has recently been extended to preparative separation where the productivity relative to the amount of resin and sol-vent used is a matter of concern. To overcome the inherent thermodynamic inefficiency of batch chromatography, as exemplified by the partial temporal usage of the resin and dilution of the product with the solvent, chromatography has been continually modified by separation engineers. Column switching and recycling represnet some of the process modifications that have brought high productivity to chromatography. Recently, the simulated moving bed (SMB) method, which claims a high separation efficiency based on counter-current moving bed chromatography. has be-come the mainstay of preparative separation, especially in chiral separation. Accordingly, this pa-per reviews the current status of SMB along with several chromatographic modification, which may be helpful in routine laboratory and industrial chromatographic practices.

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