• Title/Summary/Keyword: Calibration Curves

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Spectrophotometric Determination of Cadmium and Copper with Ammonium Pyrrolodinedithiocarbamate in Nonionic Tween 80 Micellar Media

  • Lee, Seung Gwon;Choe, Hui Seon
    • Bulletin of the Korean Chemical Society
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    • v.22 no.5
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    • pp.463-466
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    • 2001
  • The determination of Cd2+ and Cu2+ with ammonium pyrrolidinedithiocarbamate (APDC) in Tween 80 micellar media has been studied. The UV-visible spectrum of Cd(PDC)2 complex in Tween 80 media had more sensitivity tha n in chloroform. Although the UV-visible spectrum of the Cu(PDC)2 complex in Tween 80 media had somewhat less sensitivity than that in chloroform, absorbance data of Cu2+ were more reproducible in Tween 80 media. The Cd(PDC)2 and Cu(PDC)2 complexes were very stable at pH 7.0 for up to 100 minutes and could be quantitatively chelated if APDC were added to the sample solution more than 30 times the moles of Cd2+ and Cu2+ . The optimum concentration of Tween 80 was 0.1%. The calibration curves of Cd(PDC)2 and Cu(PDC)2 complexes with good linearity were obtained in 0.1% Tween 80 media. The detection limits of Cd2+ and Cu2+ were 0.0493 ㎍mL-1 and 0.0393 ㎍mL-1 , respectively. Recovery yields of Cd2+ and Cu2+ ions in the spiked real samples were almost 100%. Based on experimental results, this proposed method could be applied to the rapid and simple determination of Cd2+ and Cu2+ in real samples.

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.

Quantitative Analysis of the Seventeen Marker Components in Dangguisu-san Using Ultra-performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry (LC-MS/MS를 이용한 당귀수산 추출물 중 17종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • YAKHAK HOEJI
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    • v.58 no.3
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    • pp.158-164
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    • 2014
  • Dangguisu-san is a well-known traditional Korean herbal medicine prescription and has been widely used to treat ecchymosis, blood stagnation, and pain resulting from physical shock in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer method was established for the simultaneous determination of the 17 biomarker components in Dangguisu-san. All analytes were separated on an UPLC BEH $C_{18}$ ($100{\times}2.1$ mm, $1.7{\mu}m$) column and maintained at $45^{\circ}C$. The mobile phase consisted of two solvent systems, 0.1% (v/v) formic acid in water (A) and acetonitrile (B) by gradient flow. The injection volume was $2.0{\mu}l$ and the flow rate was 0.3 ml/min with detection at mass spectrometer. Calibration curves of the 17 biomarker components were acquired with $r^2$ values ${\geq}0.9951$. The values of limit of detection and quantification of all analytes were 0.02~6.32 ng/ml and 0.05~18.95 ng/ml, respectively. The amounts of the 17 components in Dangguisu-san sample were $3.17{\sim}13,224.50{\mu}g/g$.

Electrochemical Studies on $Sm^3+$-ARS Complexes ($Sm^3+$-ARS착물의 전기화학적 연구)

  • Son, Byoung-Chan
    • The Journal of Natural Sciences
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    • v.11 no.1
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    • pp.33-39
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    • 1999
  • Electrochemical behaviors of $Sm^3+$-ARS complexes has been investigated by d.c.polarography, differential pulse polarography and cyclic voltammetry. $Sm^3+$forms 1 : 3 adsorptive complexes with ARS.The reduction potential of complex wave $(P_2)$ shifted more negatively than the ligand wave $(P_1)$. The linear calibration curves of decreasing $P_1$ and increasing $P_2$ is obtained when $Sm^3+$ concentration varies from TEX>$2{\times}10^{-6}$ M to $3.2{\times}10^{-5}$ M.

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A hardening model considering grain size effect for ion-irradiated polycrystals under nanoindentation

  • Liu, Kai;Long, Xiangyun;Li, Bochuan;Xiao, Xiazi;Jiang, Chao
    • Nuclear Engineering and Technology
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    • v.53 no.9
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    • pp.2960-2967
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    • 2021
  • In this work, a new hardening model is proposed for the depth-dependent hardness of ion-irradiated polycrystals with obvious grain size effect. Dominant hardening mechanisms are addressed in the model, including the contribution of dislocations, irradiation-induced defects and grain boundaries. Two versions of the hardening model are compared, including the linear and square superposition models. A succinct parameter calibration method is modified to parametrize the models based on experimentally obtained hardness vs. indentation depth curves. It is noticed that both models can well characterize the experimental data of unirradiated polycrystals; whereas, the square superposition model performs better for ion-irradiated materials, therefore, the square superposition model is recommended. In addition, the new model separates the grain size effect from the dislocation hardening contribution, which makes the physical meaning of fitted parameters more rational when compared with existing hardness analysis models.

Simultaneous Determination of Avicularin and Quercitrin in Astilbe chinensis by HPLC

  • Seo, Changon;Jung, Yeon Woo;Kwon, Jin Gwan;Hong, Seong Su;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Choi, Chun Whan;Kim, Jin Kyu
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2019.04a
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    • pp.102-102
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    • 2019
  • This study developed a HPLC analysis method for the determination of avicularin (AL) and quercitrin (QT) in Astilbe chinensis by HPLC. HPLC was performed on a Capcell Pak C18 MGII column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$ and a UV detection wavelength of 254 nm. The analytical method was validated for its specificity, precision, accuracy, and linearity. The limits of detection and quantitation were AL 0.09 and 0.28 mg/mL, QT 0.03 and 0.09 mg/mL respectively. Calibration curves showed good linearity (AL r2 > 0.99990 and QT r2 > 0.99994), and the precision of analysis was satisfied (less than AL 0.59%, QT 0.63%). Recoveries of quantified compounds ranged from AL 100.57 to 102.08%, QT 99.94 to 100.64%. These results indicate that the developed HPLC method was applied successfully to the detection of AL and QT in A. chinensis.

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Analytical Method Validation of (-)Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC

  • Kwon, Jin Gwan;Jung, Yeon Woo;Seo, Changon;Hong, Seong Su;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Choi, Chun Whan;Kim, Jin Kyu
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2019.04a
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    • pp.100-100
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    • 2019
  • This study attempted to establish a High Performance Liquid Chromatography (HPLC) analysis method for the determination of (-)-epicatechin gallate as a part of the quality control for the development of functional cosmetic materials from Penthorum chinense Pursh extracts. HPLC was performed on a Unison US-C18 column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methyl alcohol at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 280 nm. The HPLC method was performed in accordance with the International Conference on Harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.11 and 0.33 mg/mL, respectively. Calibration curves showed good linearity (r2 > 0.9999), and the precision of analysis was satisfied (less than 0.6%). Recoveries of quantified compounds ranged from 99.51 to 101.92%. This result indicates that the established HPLC method is very useful for the determination of marker compound in P. chinense Pursh extracts.

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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 ($0.059{\pm}0.014%$).

Simultaneous Analysis of Four Standards of The Herbal Formula, DF-02, of Ephedra intermedia and Rheum palmatum, using by High Performance Liquid Chromatography-Ultraviolet Detector (HPLC-UVD)

  • Choi, Seong Yeon;Jeong, Birang;Jang, Hyeon Seok;Lee, Jiho;Kwon, Yong Soo;Yoon, Yoosik;Shin, Soon Shik;Yang, Heejung
    • Natural Product Sciences
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    • v.25 no.2
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    • pp.111-114
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    • 2019
  • The herbal formula, DF-02, consisting of Ephedra intermedia and Rheum palmatum are used for the treatment of the metabolic diseases such as obesity and liver fibrosis in Korean local clinics. We aimed to develop the simultaneous analytical conditions for four standards, (+)-pseudoephedrine (PSEP) and (-)-ephedrine (EP) for E. intermedia, and aloe-emodin (AE) and chrysophanol (CP) for R. palmatum using HPLC-UV techniques. The validated conditions yielded the high precision (relative standard deviation (RSD) < 3.65%) and the recoveries (94 - 106%) using the calibration curves with high linearity ($R^2$ > 0.9994). As a result, four standards of DF-02 were simultaneously determined under the developed method, which will be utilized for the quality control or evaluation of DF-02 and many herbal preparations containing E. intermedia and R. palmatum.

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.