• Title/Summary/Keyword: PDA-HPLC

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Simultaneous Analysis of Bangpungtongseong-san and Its Antioxidant Effect (방풍통성산의 동시분석 및 항산화 효능 연구)

  • Seo, Chang-Seob;Kim, Ohn Soon;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.21 no.2
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    • pp.133-143
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    • 2013
  • Objectives : We carry out the simultaneous quantification for quality control of four components in Bangpungtongseong-san (BPTSS) sample. In addition, we assessed the antioxidant effects of BPTSS sample. Methods : The used column for separation and analysis of four compounds was Luna C18 column and column oven temperature was maintained at $40^{\circ}C$. The mobile phase for simultaneous determination consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. High performance liquid chromatography-photodiode array (HPLC-PDA) method for analysis was performed at a flow rate of 1.0 mL/min with PDA detection at 254 and 280 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of BPTSS were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS) and relative electrophoretic mobility (REM). Results : Calibration curves were acquired with $r^2{\geq}0.9999$. The values of limit of detection (LOD) and quantification (LOQ) were 0.06-0.29 ${\mu}g/mL$ and 0.20-0.98 ${\mu}g/mL$, respectively. The amounts of geniposide, liquiritin, baicalin, and glycyrrhizin in BPTSS were 5.06, 7.33, 27.56, and 7.81 mg/g, respectively. The BPTSS showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction (RC50) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by CuSO4. Conclusions : The established HPLC-PDA method will be helpful to improve quality control of BPTSS. In addition, BPTSS has potentials as therapeutic agent on anti-atherosclerosis.

Simultaneous Determination of Cinnamaldehyde and Coumarin in Oryeong-san using HPLC with Photodiode Array Detector

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.18 no.2
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    • pp.251-257
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    • 2010
  • Objectives : To develop and validate High-performance liquid chromatography-photodiode array methods for simultaneous determination of two constituents in Oryeong-san(ORS). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 280 nm, were used for quantification of the two marker components of ORS. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was $H_2O$ and solvent B was acetonitrile. Results : Calibration curves were acquired with correlation coefficient ($r^2$)>0.9999, and the relative standard deviation(RSD) values(%) for intra- and inter-day precision were not exceed 1.0%. The recovery rate of each compound was in the range of 93.01-104.16%, with an RSD less than 2.0%. The contents of two compounds in ORS were 1.10-3.72 mg/g. Conclusions : The established HPLC method will be helpful to improve quality control of ORS.

Isolation of Phytochemicals from Salvia plebeia Using Countercurrent Chromatography Coupled with Reversed-phase HPLC

  • Kil, Hyun Woo;Rho, Taewoong;Seo, Young Ju;Yu, Aram;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.26 no.3
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    • pp.236-243
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    • 2020
  • Salvia plebeia R. Br. is a plant which has been used as an edible crop and traditional medicine in Asian countries. In this study, HPLC-PDA analysis and countercurrent chromatography (CCC) coupled with reversed-phase (RP) HPLC method were applied to isolate ten isolates from 3.3 g of n-butanol soluble extract from hot-water extract of S. plebeia. The use of CCC enabled us to efficiently fractionate the starting material with less sample loss and facilitate the isolation of compounds from S. plebeia extract using RP-HPLC. The isolates were determined to be caffeic acid (1), 6-hydroxyluteolin 7-O-β-D-glucoside (2), eudebeiolide B (3), (R)-rosmarinic acid (4), homoplantaginin (5), eudebeiolide D (6), plebeiolide C (7), salpleflavone (8), eupafolin (9) and hispidulin (10) based on the spectroscopic evidence.

Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Studies on the Separation and Discrimination of the Natural Yellow Pigment on Croaker (참조기 천연색소의 분리 및 판별법에 관한 연구)

  • Kim, Hee-Yun;Hong, Ki-Hyung;Hong, Jin-Hwan;Kim, Dong-Sul;Han, Sang-Bae;Lee, Eun-Ju;Lee, Jeung-Seung;Kang, Kil-Jin;Chung, Hyung-Wook;Song, Kyung-Hee;Park, Jong-Seok;Kwon, Yong-Kwan;Jang, Young-Mi;Shin, Il-Shik;Lee, Chang-Kook;Park, Hee-Yul;Ha, Sang-Chul;Jo, Jae-Sun;Park, Hye-Kyung
    • Korean Journal of Food Science and Technology
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    • v.34 no.5
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    • pp.762-769
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    • 2002
  • As a preliminary test for defining intact yellow croaker pigment, the pigment was analyzed by column chromatography and UV-vis spectrophotometry. All maximum absorbance wavelengths commonly showed three maximum absorbance ranges, similar to those of carotenoid, suggesting that the tested pigment may be carotenoid. We detected total six peak RT values in the chromatogram through PDA-HPLC under gradient mode (behavior A at 10% for initial 2 min and changed to behavior B for 60 min). Most pigments were detected at the peak with 3.27 RT value. Because seven peaks were detected under gradient mode and three under isocratic mode [methanol : methylene chloride (90 : 10, v/v)], gradient mode was determined to be more appropriate for quantitative analysis. By the comparison test of RT values among yellow pigment in croakers and reference pigments, such as zeaxanthine, ${\beta}-cryptoxanthine$, ${\beta}-carotene$, and astaxanthin, only ${\beta}-cryptoxanthine$ was detected in the white croaker, whereas such pigment of yellow croaker having RT value of 31.02 was not detected. Therefore, RT value was found to be applicable for detecting adulterated croaker.

Analytical Method of Multi-Preservatives in Cosmetics using High Performance Liquid Chromatography (HPLC 를 이용한 화장품 중 살균보존제 다성분 동시분석법 연구)

  • Min-Jeong, Lee;Seong-Soo, Kim;Yun-Jeong, Lee;Byeong-Chul, Lee
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.4
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    • pp.321-330
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    • 2022
  • This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H3PO4 addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R2) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.

Development of a Method for Analyzing the Nicotine Content in Synthetic Flavoring Substances as Unauthorized E-cigarette Liquid by Using HPLC (전자담배 액상 충진제와 유사한 합성착향료 중 니코틴의 HPLC 분석법 개발)

  • Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik;Cho, Yoon-Jae;Lee, Han-Jin;Chae, Young-Sik;Rhee, Gyu-Sik
    • Korean Journal of Food Science and Technology
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    • v.45 no.6
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    • pp.693-699
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    • 2013
  • A simple, sensitive, and specific method for quantifying the nicotine content of synthetic favoring substances (SFS) was developed using high performance liquid chromatography (HPLC) with a photo-diode array detector (PDA). Nicotine was extracted from SFS samples by using an acid-base liquid-liquid extraction method with dichloromethane and distilled water. The nicotine content was quantified by HPLC/PDA (261.9 nm) with a $C_{18}$ column under a gradient of 10% acetonitrile with 20 mM ammonium formate (ammonia solution adjusted to pH 8.7) to 100% acetonitrile. The calibration curve, analyzed from concentration standards between 0.1 to 2 mg/L, presented linearity with a correlation coefficient ($r^2$)>0.9999. The limit of quantitation (LOQ) of nicotine in SFS was 0.4 mg/kg, and the average recoveries ranged from 76.4% to 96.3%. The repeatability of measurements, expressed as the coefficient of variation (CV%), ranged from 1.74 to 5.12%. This newly developed method for nicotine quantification in SFS can be considered an analytical method with an acceptable level of sensitivity and repeatability.

Elucidation of new anti-impotency analogue in food (식품 중 발기부전치료제 유사물질 규명)

  • Suh, Junghyuck;Choi, Jangduck;Park, Kunsang;Hu, Soojung;Yoon, Taehyung;Kim, Eunju;Han, Seungwoo;Kim, Sohee;Lee, Kwangho;Kwan, Sungwon;Kim, Deukjoon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.345-353
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    • 2009
  • The new anti-impotency analogue was identified in food source. Detection of this analogue was accomplished through screening of food samples by liquid chromatography/photodiode array detector. The spectrum pattern of analogue compound was similar to that observed for hongdenafil which was analogue of sildenafil. This new compound was isolated and purified using the liquid-liquid extraction, thin layer chromatography, column chromatography and preparative HPLC. And then those structure were identified using analytical instruments such as HPLC/PDA, LC/MS/MS and NMR. The compound was given a name to oxohongdenafil which was replaced with acetyl oxoethylpiperazinyl residue instead of sulfonyl piperazine group of sildenafil. The regulation for the abovementioned analogue, oxohongdenafil, was established by Standard of Korean food code.

Determination of Pantothenic acid in Fortified Foods by HPLC (시판 영양강화식품중 판토텐산의 분석)

  • 최윤주;장재희;박혜경;박건상;구용의;황인경;김대병
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.33 no.2
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    • pp.381-385
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    • 2004
  • This study was conducted to develop an HPLC method for determining pantothenic acid in fortified foods which has typically been determined by microbiological assay (MBA) according to AOAC and Korean Food Code approved methods. Pantothenic acid was determined by reversed-phase ion-pair HPLC using UV absorption (200 nm) after extraction with 20 mM potassium phosphate solution by sonication. The recovery of spiked samples and detection limit (LOD) by HPLC were 83.5∼109.6% and 0.5 ppm (mg/kg), respectively. The LOD of the microbiological assay (MBA) was much lower than that of HPLC. The concentrations of pantothenic acid analyzed in all tested samples (n=13) confirmed compliance with declared label claims. The range of recovery ratio by the HPLC method when compared to the microbiological assay was 91.9∼117.6%. There was not significant difference (p<0.01) between the HPLC and MBA methods and the equation of the regression curve was y=1.1428x-0.2269 (r=0.9842). This proposed HPLC method for determining pantothenic acid appears to be suitable for determining pantothenic acid concentrations above 0.25 mg/100 g in fortified foods.