• Title/Summary/Keyword: HPLC-UV method

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Assays of Residual Antibiotics after Treatment of γ-ray and UV Irradiation (감마선과 UV 조사에 의한 항생제 분해)

  • Shin, Ji-Hye;Nam, Ji-Hyun;Yu, Seungho;Lee, Myunjoo;Lee, Dong-Hun
    • Journal of Radiation Industry
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    • v.4 no.1
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    • pp.39-45
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    • 2010
  • The pollution of antibiotics is a major cause of spreading antibiotics resistant bacteria in the environment. Applications of ozonation, UV, and ${\gamma}-ray$ irradiations have been introduced to remove antibiotics in the effluents from wastewater treatment system. In this study, we compared the chemical (HPLC) and biological (antimicrobial susceptibility test, AMS) assays in measuring of the concentrations of residual antibiotics after ${\gamma}-ray$ and UV irradiation. Most samples were degraded by ${\gamma}-ray$ irradiation (1~2 kGy). However, lincomycin and tetracycline were not degraded by UV irradiation. The concentration of residual antibiotics, that was treated with ${\gamma}-ray$ and UV irradiation, measuring by bioassay was similar to HPLC. The concentrations of ${\gamma}-ray$ irradiated cephradine measured by AMS test were 2 times higher than that of HPLC assay, indicating AMS test is more sensitive than HPLC assay. These results indicate that ${\gamma}-ray$ irradiation technique is more useful than UV irradiation, and biological assay is more useful to detect the antibiotics and toxic intermediates in antibiotics degradation.

Determination of DL-Carnitine Hydrochloride in Pharmaceutical Preparation by HPLC using UV Absorption Derivatives (자외부 흡광 유도체를 이용한 염산 DL-카르니틴의 분석)

  • Park, Jun-Kyu;Shin, Hee-Jong;Kim, Jung-Woo
    • Journal of Pharmaceutical Investigation
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    • v.26 no.2
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    • pp.83-89
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    • 1996
  • A reverse-phase HPLC method to determine DL-Carnitine Hydrochloride in pharmaceutical preparation is described. UV absorption derivatives of DL-Carnitine Hydrochloride were formed with p-Bromophenacyl Bromide in an essentially quantitative manner using crown ether as catalyst. The DL-Carnitine-bromophenacyl ester absorbed UV radiation strongly at 254nm, allowing the detection of as small a quantity as 12.5ng of DL-Carnitine Hydrochloride. A linear defection range was $5\;{\times}\;10-8 \;{\sim}\;5\;{\times}\;10-7M$ of DL-Carnitine Hydrochloride. And the linear regression at various drug concentration was =0.999 (n=10). The DL-Carnitine Hydrochloride in pharmaceutical preparation was successfully derivatized and separated from other constituents by reverse phase HPLC with detection at 254 nm.

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Isolation of Constituents of Lihtospermum erythrorhizon and Development of an Analytical Method of its Constituents by HPLC-UV (자근의 성분 분리 및 이들 성분의 HPLC-UV 동시분석법 개발)

  • Hong, Eun-Young;Kyung, Min-Ji;Whang, Wan-Kyunn
    • YAKHAK HOEJI
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    • v.59 no.5
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    • pp.222-229
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    • 2015
  • Lithospermi radix, the dried roots of Litospermum erythrorhizon Sieboid et Zuccarini (Boraginaceae), has long been used to treat detoxification and inflammation. In this study, we isolated two main quinoid compounds, ${\beta}$-hydroxyisovalerylshikonin (1) and acetylshikonin (2) from L. erythrorhizon. As acetylshikonin is considered as a marker compound of L. erythrorhizon, a rapid analysis method for the simultaneous determination of quinoid compounds including 2 was also developed by HPLC (High Performance Liquid Chromatography) and validation of this analytical method. By the developed method, two quinoid marker compounds (${\beta}$-hydroxyisovalerylshikonin and acetylshikonin) were successfully quantified in 31 commercial samples which were collected from different regions. The contents were 0.20% (${\beta}$-hydroxyisovalerylshikonin) and 0.22% (acetylshikonin), respectively.

Impurity Profiling and Quantification of Sudan III Dyes by HPLC-selective UV Detection

  • Yang, Ki Ryeol;Hong, Ji Yeon;Yoon, Soo Hwan;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.35 no.3
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    • pp.765-769
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    • 2014
  • An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.

Establishment of HPLC-UV Analysis Method Validation for Simultaneous Analysis of Standard Compounds of Oplopanax elatus Nakai Stem (HPLC-UV를 이용한 땃두릅나무 줄기의 지표 성분 동시 분석법 확립)

  • Yoo, Nam Ho;Kwon, Yongsoo;Kim, Myong Jo
    • Korean Journal of Pharmacognosy
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    • v.50 no.2
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    • pp.133-140
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    • 2019
  • In our previous study, we found uracil, adenosine, protocatechuic acid, syringin (eleutheroside B) and scoparone (6, 7-dimethoxycoumarin) in the Oplopanax elatus Nakai Stem. High-performance liquid chromatography (HPLC) -UV was used to quality and quantify the internal marker compounds in the O. elatus extract after validation of method with linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. The specificity assessment visually confirmed that the substance was detected without the introduction of other substances. The established method showed high linearity of the calibration curve and coefficient of correlation ($R^2$) of over the 0.999. HPLC was reported as five standard compounds equivalent using the following linear equation based on the calibration curve. The accuracy of measurement was 84.34 ~ 119.74% and the relative standard deviation (RSD) value was 0.28 ~ 1.60%. In addition, our established method showed high repeatability. The RSD value was 1.10 ~ 6.81%. So, we found the amount of the internal marker compounds in the O. elatus extract. These results demonstrated that can be used to quality evaluation of the O. elatus.

Quantitative Analysis of Kirenol in Siegesbeckia glabrescens and S. pubescens by HPLC-UV (HPLC-UV에 의한 진득찰과 털진득찰의 Kirenol 정량분석)

  • Nugroho, Agung;Lee, Kyung-Tae;Park, Hee-Juhn
    • Korean Journal of Pharmacognosy
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    • v.43 no.4
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    • pp.286-290
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    • 2012
  • Many diterpenoids from Siegesbeckia species (Compositae) and their anti-inflammatory actions have been examined. In this research, high-performance liquid chromatography-ultraviolet spectrophotometer (HPLC-UV) method was used to compare the quantitative level of kirenol (ent-pimarane-type diterpenoid) in the aerial parts of Korean S. glabrescens and S. pubescens and the Chinese Siegesbeckiae Herba. Fingerprints of the two HPLC chromatograms of Korean S. glabrescens and S. pubescens were similar, but considerably different from Chinese Siegesbeckiae Herba. The content of kirenol in S. pubescens ($16.51{\pm}0.10$ mg/ml dry weight as mean${\pm}$RSD) was higher than S. glabrescens ($13.48{\pm}0.12$ mg/g dry weight). These values were considerably higher than the Chinese Siegesbeckiae Herba ($1.55{\pm}0.74$ mg/g dry weight). Thin layer chromatography (TLC) analysis demonstrated the containing of kirenol in the three plant materials, but the presence of siegeskaurolic acid (entkaurane-type diterpenoid) only in the Chinese Siegesbeckiae Herba.

DERIVATIZATION OF FATTY ACIDS WITH 2-BROMOACETYLTRIPHENYLENE FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

  • Ryu, Jae-Ha;Park, Man-Ki
    • Analytical Science and Technology
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    • v.6 no.4
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    • pp.411-415
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    • 1993
  • A method for UV labeling of fatty acids with 2-bromoacetyltriphenylene using 18-crown-6-ether as a catalyst is described. The procedure is rapid, simple, quantitative and applicable to the HPLC analysis of fatty acids with UV detector. They have high molar absorptivity and their detection limit was about 1ng level. Nine derivatives of saturated fatty acid($C_{12}-C_{22}$) were separated on reverse-phase column(${\mu}$-Bondapak C-18) using acetonitrile-water gradient.

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Quantitative Evaluation of Radix Astragali through the Simultaneous Determination of Bioactive Isoflavonoids and Saponins by HPLC/UV and LC-ESI-MS/MS

  • Kim, Jin-Hee;Park, So-Young;Lim, Hyun-Kyun;Park, Ah-Yeon;Kim, Ju-Sun;Kang, Sam-Sik;Youm, Jeong-Rok;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.28 no.7
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    • pp.1187-1194
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    • 2007
  • The three major active isoflavonoids (calycosin-7-O-β -glucoside, isomucronulatol 7-O-β-glucoside, formononetin) and two main saponins (astragaloside I, astragaloside IV) in an extract of Radix Astragali were determined using rapid, sensitive, reliable HPLC/UV and LC-ESI-MS/MS methods. The separation conditions employed for HPLC/UV were optimized using a phenyl-hexyl column (4.6 × 150 mm, 5 μm) with the gradient elution of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm. The specificity of the peaks was determined using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source that was operated in multiple reaction monitoring (MRM) in the positive mode. 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 isoflavonoids in the extract of Radix Astragali. The results indicate that the established HPLC/UV and LC-ESI-MS/MS methods are suitable for the quantitative analysis and quality control of multi-components in Radix Astragali.

Development of Analytical Methods for Insect Moulting Hormone $({\beta}-Ecdysone)$ by HPLC/UV Using Boronate Derivatization

  • Shim, Jae-Han;Kim, In-Seon;Lim, Kye-Taek
    • Applied Biological Chemistry
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    • v.41 no.4
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    • pp.251-256
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    • 1998
  • The analytical method of ${\beta}-ecdysone$, the insect moulting hormone, by high performance liquid chromatograph (HPLC) with UV detector was developed using boronic ester derivatization and applied to the extracts of Ajuga iva, Silene otites and Schistocerca egg. Derivatization of yield with methyl-, butyl-, and phenyl-boronate was completed under mild conditions with 20-hydroxyecdysone. The conversion ratios of boronate were estimated to be 70% in methylboronic acid, 89% in butylboronic acid and 93% in phenylboronic acid. Phenylboronate showed a high sensitivity and demonstrated an effective separation on HPLC. The optimum temperature and reaction time for derivative formation were $25^{\circ}C$ and 20 min. respectively. ${\beta}-Ecdysone$ was effectively identified in extracts of Ajuga iva, Silene otites and Schistocerca egg by the HPLC method.

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Determination of Oxolinic Acid in Paddy Soil by HPLC Coupled with UV Detector (HPLC-UV검출기를 이용한 논토양 중 oxolinic acid 분석)

  • Lo, Seog-Cho;Ma, Sang-Yong;Han, Seong-Soo
    • The Korean Journal of Pesticide Science
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    • v.9 no.4
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    • pp.303-310
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    • 2005
  • This study was performed to examine analytical method of a quinolone compound, oxolinic acid in paddy soil by HPLC coupled with UV detector. Two types of soil texture in different regions were used for this experiment. Oxolinic acid was extracted by a 4 M-KOH : MeOH(1 : 3, v/v) mixtures and acidified followed by liquid-liquid partitioning in dichloromethane. Dichlormethane layer was dehydrated, evaporated and analyzed by HPLC (262 nm). Retention time was 10.2 min. The standard calibration curve of oxolinic acid showed linearity ($r^2>0.999^{**}$, y=378.99x+135.08) in the range of $1{\sim}40$ ng. The mean recoveries, evaluated from fortified soil samples at two concentration levels of 0.2 mg/kg and 1.0 mg/kg, were $90.9{\pm}4.52%$(C.V. 4.97%) and $95.0{\pm}0.23%$(C.V. 0.24%) for soil 1 and $92.2{\pm}1.15%$(C.V. 1.25%) and $93.1{\pm}0.31%$ (C.V. 0.33%) for soil 2, respectively The detection limits of two types of soils were same as 0.05 ppm. Overall, the present analytical method of oxolinic acid by HPLC coupled with UV detector seems to be used reasonably.