• Title/Summary/Keyword: HPLC-analysis

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Quantitative and Pattern Recognition Analyses for the Quality Evaluation of Cimicifugae Rhizoma by HPLC

  • Fang, Zhe;Moon, Dong-Cheul;Son, Kun-Ho;Son, Jong-Keun;Min, Byung-Sun;Woo, Mi-Hee
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.239-246
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    • 2011
  • In this study, quantitative and pattern recognition analysis for the quality evaluation of Cimicifugae Rhizoma using HPLC/UV was developed. For quantitative analysis, three major bioactive phenolic compounds were determined. The separation conditions employed for HPLC/UV were optimized using ODS $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}M$) with isocratic elution of acetonitrile and water with 0.1% phosphoric acid as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 323 nm. These methods were fully validated with respect to the linearity, accuracy, precision, recovery, and robustness. The HPLC/UV method was applied successfully to the quantification of three major compounds in the extract of Cimicifugae Rhizoma. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of twelve reference samples corresponding to five different species of Cimicifugae Rhizoma and seventeen samples purchased from markets. The results indicate that the established HPLC/UV method is suitable for the quantitative analysis and quality control of multi-components in Cimicifugae Rhizoma.

Chip-based microcapillary HPLC for proteomic analysis (칩 기반 미세관 HPLC를 이용한 단백체 분석)

  • Kim, Bo-Ra;Park, Jong-Moon;Lee, Hoo-Keun
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.407-413
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    • 2011
  • Over the last decade sophisticated and powerful microcapillary HPLC for proteomic analysis have been developed increasingly and interfaced with high resolution tandem mass spectrometers. Separation prior to mass spectrometric (MS) analysis removes impurities, and concentrates analytes in the narrow elution peaks, resulting in increased sensitivity of MS analysis. This review will focus on the recent advances of on-line highperformance separation techniques based on microfluidic chips for complex proteomic analysis.

HPLC Method Validation for Quantitative Analysis of Scopoletin from Hot-Water Extract Powder of Artemisia annua Linné (기능성 원료 인정을 위한 제출자료 작성 가이드[민원인 안내서]에 따른 개똥숙 열수추출분말의 Scopoletin 분석을 위한 HPLC 분석법 밸리데이션)

  • Kim, Seon-Hee;Yoon, Kee Dong
    • Korean Journal of Pharmacognosy
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    • v.51 no.1
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    • pp.78-85
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    • 2020
  • In this study, we shortly introduced the HPLC method validation guideline for the analysis of functional food which was released from the Ministry of Food and Drug Safety of Korea in Dec 2018. The HPLC method validation was performed through the aforementioned HPLC method validation guideline in order to quantitate scopoletin content from the hot-water extract powder of Artemisia annua Linné. The HPLC method was validated by evaluating specificity, accuracy, precision, limit of quantitation and linearity. All parameters were in the suitable ranges which are designated in the guideline, which indicated the current HPLC method is reliable to quantitate the scopoletin content from the hot-water extract of A. annua.

Investigation of Validation Guidelines for Performance Verification of High Performance Liquid Chromatograph (고성능 액체크로마토그래프 기기의 성능검증을 위한 밸리데이션 가이드라인에 대한 연구)

  • Yun, Won Nam;Lee, Beom-Gyu;Lee, Wonjae
    • YAKHAK HOEJI
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    • v.57 no.5
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    • pp.362-368
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    • 2013
  • High performance liquid chromatograph (HPLC) is the most frequently used analytical instrument in analytical laboratories for pharmaceutical analysis. In order to provide a high level of assurance for reliable data generated from the HPLC analysis, the performance qualification of the HPLC system is required. For this purpose, the performance of HPLC system should be regularly monitored by examining the key functions of the typical HPLC system (solvent delivery system, injector system, column oven, UV-VIS detector system). We have investigated the validation guidelines of the performance verification of these key modules for HPLC system. And we proposed and evaluated its validation guidelines and the related verification methods for pharmaceutical analysis that could be practically applied in Korea.

Analytical Characteristics of GC/MS and HPLC according to the Concentration Distribution of PAHs (PAHs 농도 분포에 따른 GC/MS와 HPLC의 분석특성에 관한 연구)

  • Hong, Jwa-Ryung;Choi, Kwang-Min
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.3
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    • pp.312-321
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    • 2015
  • Objectives: The purpose of this study was to determine the best method to analyze PAHs at extremely low concentrations. To this end, 16 PAHswere analyzed simultaneously by GC/MS, HPLC/FLD and HPLC/UVD, and the analytical characteristics of HPLC and GC/MS were compared. Methods: This study was conducted by GC/MS and HPLC/FLD/UVD, and evaluated linearity, precision and detection limit. Standard solutions were prepared for 21 samples in the range of $0.00001{\sim}1.0{\mu}g/mL$ and the samples were divided into four groups. All samples were made in three sets and analysis was replicated seven times. Results: Sixteen PAHs could be simultaneously separated by HPLC and GC/MS, and the adequate equipment was HPLC/FLD. The retention times by HPLC were shorter than GC/MS, and HPLC had better separation for most PAHs than GC/MS. The peaks of naphthalene and naphthalene-D8 partially overlapped for GC/MS. HPLC/FLD had a 20-2000 times lower limit of detection than GC/MS and UVD. However FLD was not adequate for analyzing acenaphthylene because it has too low a fluorescence quantum yield to be detected. The precision of HPLC/FLD/UVD and GC/MS showed less than 20% at $0.001{\mu}g/mL$ PAHs and when the concentration was higher, the coefficient of variation was decreased. HPLC/FLD was better for the overall detection of limits. Conclusions: The results indicate that the HPLC/FLD method has good linear range, precision and a detection of limits from $0.00001{\sim}0.0001{\mu}g/mL$ for all 16 PAHs. This study contributes to providing useful data for analysis technology and can be applied to occupational exposure measurement for PAHs in workplaces.

Bioactivity Analysis of Curcuminoids from Turmeric using On-line Screening HPLC-ABTS (On-line Screening HPLC-ABTS를 이용한 강황으로부터 Curcuminoids의 생물활성 분석)

  • Choi, Sun Do
    • Journal of Applied Biological Chemistry
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    • v.56 no.3
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    • pp.137-139
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    • 2013
  • Free radical scavengers in the bisdemethoxycurcumin (BDMC), demethoxycurcumin (DMC) and curcumin of turmeric (Curcuma longa) were screened, identified, quantified and isolation using coupled off-line-2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) and on-line screening high-performance liquid chromatography (HPLC)-ABTS assay. There was a very small margin of error between the off-line-ABTS method and the on-line screening HPLC-ABTS method.

Quantitative Analysis for the Quality Evaluation of Scutellariae Radix by HPLC/UVD

  • Jeong, Su-Yang;Moon, Dong-Cheul;Son, Kun-Ho;Son, Jong-Keun;Min, Byung-Sun;Woo, Mi-Hee
    • Natural Product Sciences
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    • v.17 no.4
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    • pp.321-327
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    • 2011
  • In this study, quantitative analysis was developed using HPLC/UVD for the quality evaluation of Scutellariae Radix. For quantitative analysis, six major bioactive compounds were assessed. The separation conditions employed for HPLC/UVD were optimized using Phenomenex $C_{18}$ column ($250{\times}4.6$ mm, 5 ${\mu}m$) with a gradient of solvent A (1% acetic acid of $H_2O$) and solvent B (acetonitrile : methanol : acetic acid = 70 : 30 : 1) as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 275 nm. These methods were fully validated with respect to linearity, accuracy, precision and recovery. The HPLC/UVD method was applied successfully to the quantification of six major compounds in the extract of Scutellariae Radix. The results indicate that the established HPLC/UVD method is suitable for the quantitative analysis and quality control of multicomponents in Scutellariae Radix.

Analysis of Carbendazim and Carbaryl by Micro-HPLC (Micro-HPLC에 의한 Carbendazim과 Carbaryl의 분석)

  • Choi, Kyoung-Sook;Lee, Hoe-Yeon;Lee, Duck-Hee;Byun, Woon-Ki
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.421-425
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    • 1994
  • A micro-high performance liquid chromatography(Micro-HPLC) techniquie with solid phase extraction was reported which detected carbendazim and carbaryl at picogram levels. They were separated on microbore packed $C_{18}$ column($1.0mm\;I.\;D{\times}150mm$, $d_f=5{\mu}m$) using a 50% methanol mobile phase and detected at UV 220nm(${\alpha}=2.94$, $R_s=4.71$), while they were not resolved on analtical HPLC system(${\alpha}=1.27$, $R_s=0.76$). The detection thresholds of carbendazim and carbaryl were 0.5ng and 0.1ng on Micro-HPLC, therefore Micro-HPLC system was 20~40 told more sensitive than anayltical HPLC system. Sep-Pak $C_{18}$ catridge was found to be efficient in enriching carbendazim and carbaryl from dilute aqueous solution with 97.0% and 97.8% recoveries of them. The Sep-Pak $C_{18}$ catridge followed by the Micro-HPLC had been applied to the quantitative analysis of carbendazim and carbaryl in spiked juices and a commercial drinking water.

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A Study on the Separation of n-Hexane by Molecular Sieve 5A and the Purification for HPLC use (분자체 5A를 이용한 n-헥산의 분리와 HPLC급으로의 정제에 관한 연구)

  • Choi, Beom Suk;Kim, Young Man;Kim, Sun Tae
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.21-27
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    • 1993
  • Technical grade n-hexane whose purity is 54% has been purified for HPLC use. Methylcyclopentane, 2-methylpentane, and 3-methylpentane which are hardly isolated by fractional distillation were separated by the liquid-solid chromatography using molecular sieve 5A. UV and fluorescence impurities whose contents are critically regulated for HPLC solvent were removed by the adsorptive separation with alumina and silica gel. The present method also reduced the impurities of color(APHA), acidity, water, residue after evaporation, sulfur, and thiophene content, and the impurity contents were well within the specifications of HPLC solvent.

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Quantitative Analysis of Glycine Semen Nigra and Eucommiae Cortex for Standardization of GCSB-5 Preparation (생약복합제 GCSB-5의 품질 표준화를 위한 흑두 및 두충의 함량 분석)

  • Lee, Eun-Hee;Cha, Bae-Cheon
    • Korean Journal of Pharmacognosy
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    • v.40 no.1
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    • pp.18-24
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    • 2009
  • GCSB-5 preparation is a purified extract from a mixture six herbal medicines (Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used in traditional medicine to treat various bone disorders. This study was carried out to obtain the HPLC analysis method that can be used to establish quantitative analysis of Glycine Semen Nigra and Eucommiae Cortex for standardization of GCSB-5 preparation. HPLC analysis methods for the simultaneous determination of genistin (Glycine Semen Nigra) and geniposide (Eucommiae Cortex) were established for the quality control of herbal medicinal raw material and preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline. As the result of quantitative analysis, the contents of genistin and geniposide in the raw material of GCSB-5 preparation were 0.0426-0.0427 mg/g and 0.431-0.432 mg/g. And GCSB-5 preparation contained genistin of 0.0202-0.0203 mg/capsule and geniposide of 0.211-0.212 mg/capsule, respectively.