• Title/Summary/Keyword: HPLC separation

Search Result 461, Processing Time 0.027 seconds

Simultaneous Analysis of Six Constituents in Oyaksungi-san using HPLC-PDA (HPLC-PDA를 이용한 오약순기산 중 6종 성분의 동시분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Herbal Formula Science
    • /
    • v.20 no.2
    • /
    • pp.37-46
    • /
    • 2012
  • Objectives : Oyaksungi-san(Wuyaoshunqisan) has been used for treatment of stroke and rheumatoid arthritis in Korea. In this study, a simple and accurate high-performance liquid chromatography(HPLC) method was established for simultaneous determination of six main components, liquiritin, ferulic acid, naringin, hesperidin, neohesperidin, and glycyrrhizin in Oyaksungi-san, a traditional Korean herbal prescription. Methods : The analytical column for separation of six constituents was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of two solvent systems, 1.0% (v/v) acetic acid in $H_2O$ (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient flow. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254 nm for glycyrrhizin, 280 nm for liquiritin, naringin, hesperidin, and neohesperidin, and 320 nm for ferulic acid. Results : Calibration curves were acquired with $r^2$ values ${\geq}0.9998$. The results of recovery test were 91.58%-105.90% with a relative standard deviations (RSDs, %) value less than 2.0%. The values of RSD for intra- and inter-day precision were 0.03%-1.72% and 0.03%-1.63%, respectively. The contents of the six compounds in Oyaksungi-san were 0.33-9.30 mg/g. Conclusions : The newly established HPLC method will be helpful to improve quality control of Oyaksungi-san.

Determination of nadolol enantiomers in human plasma using a coupled achiral-chiral high-performance liquid chromatography method

  • Lee, Seung-Beom;Pham, Thuy-Vy;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Nguyen, Thi-Ngoc-Van;Kang, Jong-Seong;Mar, Woongchon;Kim, Kyeong Ho
    • Analytical Science and Technology
    • /
    • v.33 no.2
    • /
    • pp.59-67
    • /
    • 2020
  • Nadolol is a β-blocker drug, which effectively manages hypertension and angina pectoris. Its chemical structure allows the formation of four possible stereoisomers. A coupled column high-performance liquid chromatographic (HPLC) system with UV and fluorescence detection was investigated for simultaneously determining four nadolol enantiomers in human plasma. The plasma samples were prepared using a convenient liquid-liquid extraction process and passed through HPLC. Nadolol was initially separated from the endogenous compounds or other impurities in human plasma on a Phenomenex silica column, and its enantiomers were resolved and determined on a Chirapak AD-H column. The developed HPLC method achieved an effective chiral separation and significantly eliminated endogenous compound interference. This optimal HPLC method was validated following FDA guidelines. The results showed good selectivity, linearity, accuracy (90.50 % - 105.27 %), and precision (RSDs < 9.52 %) for each enantiomer. This method was also successfully applied to determine nadolol enantiomers in the plasma samples of a healthy male volunteer (after orally administering 80 mg racemic nadolol), proving its suitability for nadolol stereoselective pharmacokinetic studies.

HPLC-based metabolic profiling and quality control of leaves of different Panax species

  • Yang, Seung-Ok;Lee, Sang Won;Kim, Young Ock;Sohn, Sang-Hyun;Kim, Young Chang;Hyun, Dong Yoon;Hong, Yoon Pyo;Shin, Yu Su
    • Journal of Ginseng Research
    • /
    • v.37 no.2
    • /
    • pp.248-253
    • /
    • 2013
  • Leaves from Panax ginseng Meyer (Korean origin and Chinese origin of Korean ginseng) and P. quinquefolius (American ginseng) were harvested in Haenam province, Korea, and were analyzed to investigate patterns in major metabolites using HPLC-based metabolic profiling. Partial least squares discriminant analysis (PLS-DA) was used to analyze the the HPLC chromatogram data. There was a clear separation between Panax species and/or origins from different countries in the PLS-DA score plots. The ginsenoside compounds of Rg1, Re, Rg2, Rb2, Rb3, and Rd in Korean leaves were higher than in Chinese and American ginseng leaves, and the Rb1 level in P. quinquefolius leaves was higher than in P. ginseng (Korean origin or Chinese origin). HPLC chromatogram data coupled with multivariate statistical analysis can be used to profile the metabolite content and undertake quality control of Panax products.

Separation of liquiritin, glycyrrhizic acid and glabridin from licorice by RP-HPLC (RP-HPLC를 이용한 감초에서 liquiritin, glycyrrhizic acid, glabridin의 분리)

  • Tian, Minglei;Yan, Hongyuan;Row, Kyung Ho
    • Analytical Science and Technology
    • /
    • v.21 no.2
    • /
    • pp.102-108
    • /
    • 2008
  • Reversed-phase high performance liquid chromatography (RP-HPLC) was used for the simultaneous determination of liquiritin (LQ), glycyrrhizic acid (GA) and glabridin from licorice. An optimized run condition was selected with a binary gradient elution of methanol-water which ramped 35/65 to 80/20 (vol. %) in 0.0-8.0 min and a flow rate of 1.0 mL/min. A good linearity was obtained between 0.2 mg/mL and 1.0 mg/mL for LQ and GA, and 0.01 mg/mL-0.2 mg/mL for glabridin with the relative standard deviations less than 0.90% (n=5). The developed method was successfully applied to determination of the three components from licorice samples. The mean recoveries of three components are 80.79% for liquiritin, 89.71% for glycyrrhizic acid and 72.50% for glabridin.

Determination of Coccidiostats (Amprolium and Decoquinate) in Cattle and Chicken's Muscle using High Performance Liquid Chromatography

  • Kim, Byung-Ju;Ham, Hyun-Sun;Lee, Jin-Joo;Cheong, Nam-Yong;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
    • /
    • v.33 no.2
    • /
    • pp.559-563
    • /
    • 2012
  • An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

Discrimination between steam processed and unprocessed Tubers of Gastrodia elata Blume by HPLC

  • Zhao, Bing Tian;Song, Si Whan;Le, Duc Dat;Ma, Eun Sook;Son, Jong Keun;Woo, Mi Hee
    • Analytical Science and Technology
    • /
    • v.32 no.6
    • /
    • pp.217-224
    • /
    • 2019
  • In this study, to evaluate the effectiveness and safety of oral therapy using Gastrodiae Rhizoma, a new HPLC-PDA analysis method was developed for the simultaneous quantitation of the three major components: (1) gastrodin, (2) gastrodigenin, and (3) p-hydroxybenzaldehyde, in steam processed and unprocessed tubers of Gastrodia elata Blume. The clear separation of the three components was achieved on a C18 column (250 × 4.6 mm, 5 ㎛) by gradient elution using water (including 0.1 % formic acid) and acetonitrile as the mobile phase. The flow rate was 1.0 mL/min, and the UV detector wavelength was set at 270 nm. The results demonstrate satisfactory linearity, recovery, precision, accuracy, stability, and robustness. The established HPLC-PDA method was applied to quantify three major compounds in 59 samples of G. elata Blume tubers. Finally, the steam processed and unprocessed tubers of G. elata Blume were successfully distinguished by pattern recognition analysis.

Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs (MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석)

  • 서계원;이재일;이채용;이정치
    • Journal of Food Hygiene and Safety
    • /
    • v.18 no.2
    • /
    • pp.43-50
    • /
    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

Determination of Tocopherol Contents in Refined Edible Oils Using an HPLC Method

  • Hu, Jiang-Ning;Zhu, Xue-Mei;Adhikari, Prakash;Li, Dan;Kim, In-Hwan;Lee, Ki-Teak
    • Preventive Nutrition and Food Science
    • /
    • v.14 no.3
    • /
    • pp.260-264
    • /
    • 2009
  • A high-performance liquid chromatography method was applied to determine the contents of tocopherols in edible oils using a LiChrosorb DIOL HPLC column and hexane fortified with 0.1% acetic acid in an isocratic mode. The validation of the method included tests for linearity, sensitivity, accuracy, precision, and recovery. All calibration curves showed good linear regression ($r^2$>0.9995) within the tested ranges. The established method offered good precision and accuracy with overall intra-day and inter-day variations of 0.94$\sim$4.27 and 1.77$\sim$ 4.88%, respectively. The tocopherol recoveries ranged from 91.44$\sim$108.90%. Subsequently, the method was successfully applied to qualitatively and quantitatively determine the total contents of $\alpha$, $\gamma$, and $\delta$-tocopherols in 12 selected refined edible oils, showing a range of 0.92 to 188.71 mg/100 g.

The Assessment of Carbendazim, Cyazofamid, Diethofencarb and Pyrimethanil Residue Levels in P. ginseng (C. A. Meyer) by HPLC

  • Choi, Jeong-Heui;El-Aty, A.M.Abd;Park, Young-Seok;Cho, Soon-Kil;Shim, Jae-Han
    • Bulletin of the Korean Chemical Society
    • /
    • v.28 no.3
    • /
    • pp.369-372
    • /
    • 2007
  • A fast and simple high-performance liquid chromatography (HPLC) method for the simultaneous determination of four pesticides having fungicide properties has been proposed for Panax ginseng, C. A. Meyer grown for 4, 5, or 6 years. Analytical separation was performed on C18 columns using ultraviolet detector under gradient conditions. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The HPLC response for all pesticides was linear, with determination coefficients > 0.9986. The average rate of recovery for pesticides spiked with 2 fortification levels was > 72% with relative standard deviations < 9%. The limits of quantification (LOQ) ranged from 0.03 to 0.16 ppm. These LOQs were lower than the respective maximum residue limits (MRL) established by the Korean Food and Drug Administration (KFDA), except for cyazofamid. The proposed method was used to determine pesticide residue levels in samples of ginseng obtained from Jeonnam Province (Republic of Korea). None of the pesticides were found in ginseng samples grown for 4, 5, or 6 years.

Composition Studies on the Aromatic Tobacco Varieties (Nicotiana tabacum L.): 1. Characteristics of Less-Volatile Organic Components. (향끽미종 잎담배 성분조성에 관한 연구 1. 휘발성이 적은 유기성분의 특성조사)

  • Kim, Kyoung-Rae;Park, Jeen-Woo;Lee, Un-Chul;Heu, Il
    • Journal of the Korean Society of Tobacco Science
    • /
    • v.2 no.2
    • /
    • pp.1-7
    • /
    • 1980
  • Less-volatile organic components in leaves from aromatic tobaccos of different varieties, both Oriental and Korean types were isolated and concentrated using a simple apparatus with fewer manipulations. Each less-volatile concentrate was then subjected to spectrophotometric recording in the visible range, to thin-layer chromatographic group separation, and high-performance liquid chromatographic profile analysis. The methods allow detection of significant quantitative differences in visible absorption spectra, TLC patterns, and high resolution HPLC profiles among varieties.

  • PDF