• Title/Summary/Keyword: Inter-calibration

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An HPLC method for the determination of thioctic acid in raw material and tablets

  • Mai, Xuan-Lan;Ahn, GyeChan;Lee, SeokHan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.221-225
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    • 2017
  • Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Feature Based Multi-Resolution Registration of Blurred Images for Image Mosaic

  • Fang, Xianyong;Luo, Bin;He, Biao;Wu, Hao
    • International Journal of CAD/CAM
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    • v.9 no.1
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    • pp.37-46
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    • 2010
  • Existing methods for the registration of blurred images are efficient for the artificially blurred images or a planar registration, but not suitable for the naturally blurred images existing in the real image mosaic process. In this paper, we attempt to resolve this problem and propose a method for a distortion-free stitching of naturally blurred images for image mosaic. It adopts a multi-resolution and robust feature based inter-layer mosaic together. In each layer, Harris corner detector is chosen to effectively detect features and RANSAC is used to find reliable matches for further calibration as well as an initial homography as the initial motion of next layer. Simplex and subspace trust region methods are used consequently to estimate the stable focal length and rotation matrix through the transformation property of feature matches. In order to stitch multiple images together, an iterative registration strategy is also adopted to estimate the focal length of each image. Experimental results demonstrate the performance of the proposed method.

Quantitation of Mevinolinic Acid in Human Plasma by HPLC (고속액체크로마토그래피를 이용한 사람 혈장중 메비놀린 산의 정량)

  • Oh, Han-Suk;Park, Dong-Young;Seo, Sung-Hoon;Kim, Young-Gwan;Hong, Seon-Pyo;Choi, Young-Wook;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.30 no.4
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    • pp.279-282
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    • 2000
  • Simple and precise high-performance liquid chromatographic (HPLC) assay was developed and validated for the determination of a HMG-CoA reductase inhibitor, $lovastatin^{TM}$ and its active metabolite (mevinolinic acid) in human plasma. The method involved solid phase extraction of mevinolinic acid and internal standard using Sep-Pak Cartridge. Samples were analyzed by reversed-phase HPLC using $Capcell-Pak\;C_{18}$ column with ultraviolet detection at 238 nm. The quantitation limit of mevinolinic acid was 2 ng/ml and the calibration curve was linear over the range of 2-50 ng/ml $(r^2>0.999)$ with human plasma. The analyses of quality control samples indicated that the normal values could be predicted with an accuracy >97%. The intra- and inter-day coefficients of variation for the analyses were <10%. The average recoveries were similar (79%) for mevinolinic acid and methylmevinolinic acid. The method described has been successfully applied to the quantification of mevinolinic acid in about 1,000 human plasma samples over six-month period.

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Simultaneous Analysis of Liquiritin and Glycyrrhizin in Sagunja-tang by HPLC-PDA (HPLC-PDA에 의한 사군자탕 중 Liquiritin과 Glycyrrhizin의 동시분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.42 no.3
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    • pp.240-245
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    • 2011
  • A high-performance liquid chromatography (HPLC) method was developed for quantitative analysis of liquiritin and glycyrrhizin in Sagunja-tang (SGT, Sijunzi-tang in Chinese), a traditional Korean medicine. HPLC analysis was performed using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 254 nm and 280 nm for quantification of the two components in SGT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Calibration curves were acquired with $r^2$ values > 0.9998, and the relative standard deviations (RSDs, %) for intra- and inter-day precision were not exceed 4.0%. The recovery of each component was in the range of 91.85 - 108.62%, with a RSD less than 4.0%. The contents of the two components in SGT were 7.94 - 13.83 mg/g.

Development of Sensitive Analytical Method of Rhodanthpyrone A by a LC-MS/MS and its Application to Bioavailability Study in Rats

  • Kang, Bitna;Yoon, Jeong A;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.10 no.3
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    • pp.88-92
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    • 2019
  • A sensitive analytical method of rhodanthpyrone A in rat plasma was developed using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Rhodanthpyrone A and rhodanthpyrone B (internal standard) in rat plasma were extracted by a liquid-liquid extraction method with ethyl acetate. This extraction method gave results in high and reproducible extraction recovery in the range of 73.75-79.90% with no interfering peaks around the peak elution time of rhodanthpyrone A and B. The standard calibration curves for rhodanthpyrone A ranged from 0.5 to 2000 ng/mL were linear with $r^2$ > 0.994 and the inter- and intra-day accuracy and precision and the stability were within acceptance criteria. Using this validated analytical method, pharmacokinetics of rhodanthpyrone A following intravenous and oral administration of rhodanthpyrone A at doses of 2 mg/kg and 30 mg/kg, respectively, were investigated. Rhodanthpyrone A in rat plasma showed multi-exponential elimination pattern with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 3.7%. Collectively, the newly developed sensitive LC-MS/MS analytical method of rhodanthpyrone A could be successfully applied to investigate the pharmacokinetic properties of this compound and would be useful for the further studies on the efficacy, toxicity, and biopharmaceutics of rhodanthpyrone A.

Correlation between parameters of pulse-type motions and damage of low-rise RC frames

  • Cao, Vui Van;Ronagh, Hamid Reza
    • Earthquakes and Structures
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    • v.7 no.3
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    • pp.365-384
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    • 2014
  • The intensity of a ground motion can be measured by a number of parameters, some of which might exhibit robust correlations with the damage of structures subjected to that motion. In this study, 204 near-fault pulse-type records are selected and their seismic parameters are determined. Time history and damage analyses of a tested 3-storey reinforced concrete frame representing for low-rise reinforced concrete buildings subjected to those earthquake motions are performed after calibration and comparison with the available experimental results. The aim of this paper is to determine amongst several available seismic parameters, the ones that have strong correlations with the structural damage measured by a damage index and the maximum inter-story drift. The results show that Velocity Spectrum Intensity is the leading parameter demonstrating the best correlation, followed by Housner Intensity, Spectral Acceleration and Spectral Displacement. These seismic parameters are recommended as reliable parameters of near-fault pulse-type motions related to damage potential of low-rise reinforced concrete structures. The results also reaffirm that the conventional and widely used parameter of Peak Ground Acceleration does not exhibit a good correlation with the structural damage.

Isolation and Quantitative Analysis of Naringenin, Sakuranetin and Prunetin from the Barks of Prunus yedoensis (왕벚나무 껍질로부터 Naringenin, Sakuranetin, Prunetin의 분리 및 함량 분석)

  • Kim, Eun-Nam;Kim, Sung-Cheol;Jeong, Gil-Saeng
    • Korean Journal of Pharmacognosy
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    • v.50 no.3
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    • pp.226-231
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    • 2019
  • Prunus yedoensis Matsum. (Rosaceae) has been used for cough, urticaria, pruritus, dermatitis, asthma and relaxation in traditional Korean medicine. In this study, naringenin, sakuranetin and prunetin were isolated from the barks of P. yedoensis and quantification were performed by using high performance liquid chromatography (HPLC) method with diode array detector. The structures of naringenin and sakuranetin, prunetin were identified NMR spectroscopic data analysis. The content of each compound was analyzed by HPLC and the analytical method was validated through linearity, precision, accuracy and specificity test. The result showed that calibration curves of three compounds naringenin, sakuranetin and prunetin indicated great linearity with a correlation coefficient ($R^2$) of 1.00, 1.00 and 0.99. Intra and inter day measurement accuracy of the three compounds ranged from 92.70 ~ 112.70%, and showed precision was less than 3%. Therefore, the content analysis showed that naringenin ($0.132{\pm}0.016%$), sakuranetin ($0.108{\pm}0.023%$), and prunetin ($0.059{\pm}0.014%$).

Isolation and Quantitative Analysis of Cudratricusxanthone A and Cudraxanthone D from Roots of Cudrania tricuspidata Bureau (꾸지뽕나무 뿌리로부터 Cudratricusxanthone A와 Cudraxanthone D의 분리 및 함량 분석)

  • Park, Soo-Yeun;Kim, Eun-Nam;Jeong, Gil-Saeng
    • Korean Journal of Pharmacognosy
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    • v.50 no.1
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    • pp.59-64
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    • 2019
  • Cudrania tricuspidata Bureau (Moraceae) has been used for physical weakness, impotence and insomnia in traditional Korean medicine. In this study, cudratricusxanthone A and cudraxanthone D were isolated from roots of C. tricuspidata and quantification were achieved by using high performance liquid chromatography (HPLC) method with diode array detector. The isolated compound was identified by NMR analysis and HPLC method was validated by linearity, precision and specificity test. The results showed that calibration curves of two compounds indicated great linearity with a correlation coefficient ($R^2$) of 0.9976 and 0.9995. The limits of detection (LOD) for cudratricusxanthone A and cudraxanthone D were 1.15, $0.11{\mu}g/ml$. Intra-day precision of cudratricusxanthone A and cudraxanthone D were 0.32~1.99%, 0.09~3.32% and inter-day precision were 0.59~2.40%, 0.28~1.55% RSD (%) values, respectively. The specificity was confirmed by chromatograph and quantitative contents of cudratricusxanthone A and cudraxanthone D were $0.46{\pm}0.02%$ and $1.53{\pm}0.06%$. Therefore, this study can be used as a basic research data for the quantitative analysis of derived compounds from roots of C. tricuspidata.

Simultaneous Determination of α-Amanitin and β-Amanitin in Mouse Plasma Using Liquid Chromatography-High Resolution Mass Spectrometry

  • Bang, Young Yoon;Lee, Min Seo;Lim, Chang Ho;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • v.12 no.3
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    • pp.112-117
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    • 2021
  • α-Amanitin and β-amanitin are highly toxic bicyclic octapeptides responsible for the poisoning of poisonous mushrooms such as Amanita, Galerina, and Lepiota by inhibiting RNA polymerase II, DNA transcription, and protein synthesis. A sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using parallel reaction monitoring mode was developed and validated for the simultaneous determination of α- and β-amanitin in mouse plasma to evaluate the toxicokinetics of α- and β-amanitin in mice. Protein precipitation of 5 μL mouse plasma sample with methanol as sample clean-up procedure and use of negative electrospray ionization resulted in better sensitivity and less matrix effect. The calibration curves for α- and β-amanitin in mouse plasma were linear over the range of 0.5-500 ng/mL. The intra- and inter-day coefficient of variations and accuracies for α- and β-amanitin at four quality control concentrations were 3.1-14.6% and 92.5-115.0%, respectively. The present method was successfully applied to the toxicokinetic study of α- and β-amanitin after an oral administration of α- and β-amanitin at 1.5 mg/kg dose to male ICR mice.

Development and validation of an analytical method to quantify baphicacanthin A by LC-MS/MS and its application to pharmacokinetic studies in mice

  • Jeon, So Yeon;Kim, San;Park, Jin-Hyang;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Analytical Science and Technology
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    • v.35 no.2
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    • pp.60-68
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    • 2022
  • In this study, we developed and validated a sensitive analytical method to quantify baphicacanthin A in mouse plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard calibration curves for baphicacanthin A ranged from 0.5 to 200 ng/mL and were linear, with an r2 of 0.985. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. Besides, we investigated the pharmacokinetics of baphicacanthin A following its intravenous (5 mg/kg) and oral administration (30 mg/kg). Intravenously injected baphicacanthin A showed biphasic elimination kinetics with high clearance and volume of distribution values. Furthermore, baphicacanthin A showed a rapid absorption but low aqueous solubility (182.51±0.20 mg/mL), resulting in low plasma concentrations and low oral bioavailability (2.49 %). Thus, we successfully documented the pharmacokinetic properties of baphicacanthin A using this newly developed sensitive LC-MS/MS quantification method, which could be used in future lead optimization and biopharmaceutic studies.