• Title/Summary/Keyword: precision validation

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Variation of Saponin Content in the Decoctions of Platycodi Radix (II) (길경(桔梗)의 추출조건에 따른 사포닌함량의 변화 (제2보))

  • Yoo, Dae-Seok;Choi, Yeon-Hee;Cha, Mi-Ran;Choi, Chun-Whan;Kim, Mi-Ri;Yon, Gyu-Hwan;Hong, Kyung-Sik;Lee, Byung-Hoe;Kim, Eun-Ju;Cho, Sang-Wook;Kim, Young-Sup;Ryu, Shi-Yong;Kang, Jong-Seong
    • Korean Journal of Pharmacognosy
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    • v.41 no.2
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    • pp.147-152
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    • 2010
  • The capability of the solvents for extracting the bioactive saponins from the roots of Platycodon grandiflorum (Campanulaceae) was investigated to obtain an ideal extract which contained bioactive saponins with high quality and high quantity. The content of eight representative saponins in extracts, such as deapioplatycoside E, platycoside E, platyconic acid A and platycodin D, platycodin $D_3$, platycodin $D_2$, polygalacin $D_2$, polygalacin D were analyzed simultaneousely by the modified HPLC analytical method. The validation test of the modified qualitative and quantitative analytical method employing the ELSD equipped HPLC for eight representative saponins in the roots extract of P. grandiflorum showed a good linearity, precision and accuracy. the correlation coefficient ($r^2$) values of the calbration curves for each saponins were observed to be over 0.9990. LOD and LOQ of each saponin was calculated as $0.10{\mu}g{\sim}0.40{\mu}g$ (LOD) and $0.40{\mu}g{\sim}0.80{\mu}g$ (LOQ), respectively. Recovery rates of each saponin were also calculated as over 98%, respectively. With exception of two saponins, platyconic acid A and platycodin D, The content of eight saponins in extracts was decreased proportionally to the increment of the water ratio of solvent for extraction. Consequently, as aquous alcohol was used as a solvent for extracting the saponin components from powdered roots of P. grandiflorum, the water content in the aquous alcohol was seemed to be a critical factor for extracting efficacy. The 60-80% ratio of alcohol in the aquous alcohol were deduced to be suitable and recommendable for the preparation of roots extract of P. grandiflorum which contained saponins with high quality and high quantity.

Determination of Ethambutol n Human Plasma by a Validated HPLC Method and Its Application to Single-dose Pharmacokinetics (인체혈장 중 에탐부톨의 HPLC 분석법의 검증 및 단일용량 투여에 의한 약물동태 연구)

  • Gwak, Hey-Sun;Park, Kyung-Ho;Choi, Jun-Shik;Song, Gin-A;Sung, Min-Kyung;Jang, Jung-Ok;Lee, Hwa-Jeong
    • Journal of Pharmaceutical Investigation
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    • v.35 no.2
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    • pp.123-127
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    • 2005
  • An HPLC method was employed for the determination of ethambutol in human plasma. After addition of internal standard (IS, octylamine, $2\;{\mu}g/mL$) and alkalinization of the plasma with 5 M sodium hydroxide, the drug and IS were extracted into the mixture of chloroform and diethyl ether (40:60, v/v). Following a 15-min vortex-mixing and a 10min centrifugation, the organic phase was spiked with $100{\mu}L$ of phenylethylisocyanate $(2000{\mu}g/mL)$ for chemical derivatization, mixed for 5 min and evaporated to dryness under a stream of nitrogen. The residue was reconstituted with $100{\mu}L$ of mobile phase and $20{\mu}L$ was injected into C18 column with a mobile phase consisting of methanol:water (70:30, v/v). The samples were detected utilizing an ultraviolet detector at 200 nm. The method was specific and validated with a limit of $0.15\;{\mu}g/mL$. Intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification. The applicability of this method was demonstrated by analysis of human plasma after oral administration of a single 1200-mg dose to 20 healthy subjects. From the plasma ethambutol concentration vs. time curves, the mean AUC was $9.61{\pm}1.64\;{\mu}g{\cdot}hr/mL$ and Cmax of $2.68\;{\mu}g/mL$ reached 2.73 hr after administration. The mean biological half-life of ethambutol was $3.46{\pm}1.21$ hr. Based on the results, this simple and validated assay could readily be used in any pharmacokinetic studies using humans.

Integrating UAV Remote Sensing with GIS for Predicting Rice Grain Protein

  • Sarkar, Tapash Kumar;Ryu, Chan-Seok;Kang, Ye-Seong;Kim, Seong-Heon;Jeon, Sae-Rom;Jang, Si-Hyeong;Park, Jun-Woo;Kim, Suk-Gu;Kim, Hyun-Jin
    • Journal of Biosystems Engineering
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    • v.43 no.2
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    • pp.148-159
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    • 2018
  • Purpose: Unmanned air vehicle (UAV) remote sensing was applied to test various vegetation indices and make prediction models of protein content of rice for monitoring grain quality and proper management practice. Methods: Image acquisition was carried out by using NIR (Green, Red, NIR), RGB and RE (Blue, Green, Red-edge) camera mounted on UAV. Sampling was done synchronously at the geo-referenced points and GPS locations were recorded. Paddy samples were air-dried to 15% moisture content, and then dehulled and milled to 92% milling yield and measured the protein content by near-infrared spectroscopy. Results: Artificial neural network showed the better performance with $R^2$ (coefficient of determination) of 0.740, NSE (Nash-Sutcliffe model efficiency coefficient) of 0.733 and RMSE (root mean square error) of 0.187% considering all 54 samples than the models developed by PR (polynomial regression), SLR (simple linear regression), and PLSR (partial least square regression). PLSR calibration models showed almost similar result with PR as 0.663 ($R^2$) and 0.169% (RMSE) for cloud-free samples and 0.491 ($R^2$) and 0.217% (RMSE) for cloud-shadowed samples. However, the validation models performed poorly. This study revealed that there is a highly significant correlation between NDVI (normalized difference vegetation index) and protein content in rice. For the cloud-free samples, the SLR models showed $R^2=0.553$ and RMSE = 0.210%, and for cloud-shadowed samples showed 0.479 as $R^2$ and 0.225% as RMSE respectively. Conclusion: There is a significant correlation between spectral bands and grain protein content. Artificial neural networks have the strong advantages to fit the nonlinear problem when a sigmoid activation function is used in the hidden layer. Quantitatively, the neural network model obtained a higher precision result with a mean absolute relative error (MARE) of 2.18% and root mean square error (RMSE) of 0.187%.

Development of Analytical Method for Determination of Baicalin, Eleutheroside E, and Ligustilide by LC-MS/MS in Raw Materials of Health Functional Foods (LC-MS/MS를 이용한 건강기능식품 원료 중 바이칼린, 엘레우테로사이드 E, 리구스틸라이드 동시분석법 개발)

  • Keum, Eun Hee;Chung, So Young;Lee, Jin Hee;Kim, Meehye
    • Journal of Food Hygiene and Safety
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    • v.32 no.3
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    • pp.193-198
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    • 2017
  • Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

Prospective validation of a novel dosing scheme for intravenous busulfan in adult patients undergoing hematopoietic stem cell transplantation

  • Cho, Sang-Heon;Lee, Jung-Hee;Lim, Hyeong-Seok;Lee, Kyoo-Hyung;Kim, Dae-Young;Choe, Sangmin;Bae, Kyun-Seop;Lee, Je-Hwan
    • The Korean Journal of Physiology and Pharmacology
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    • v.20 no.3
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    • pp.245-251
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    • 2016
  • The objective of this study was to externally validate a new dosing scheme for busulfan. Thirty-seven adult patients who received busulfan as conditioning therapy for hematopoietic stem cell transplantation (HCT) participated in this prospective study. Patients were randomized to receive intravenous busulfan, either as the conventional dosage (3.2 mg/kg daily) or according to the new dosing scheme based on their actual body weight (ABW) ($23{\times}ABW^{0.5}mg\;daily$) targeting an area under the concentration-time curve (AUC) of $5924{\mu}M{\cdot}min$. Pharmacokinetic profiles were collected using a limited sampling strategy by randomly selecting 2 time points at 3.5, 5, 6, 7 or 22 hours after starting busulfan administration. Using an established population pharmacokinetic model with NONMEM software, busulfan concentrations at the available blood sampling times were predicted from dosage history and demographic data. The predicted and measured concentrations were compared by a visual predictive check (VPC). Maximum a posteriori Bayesian estimators were estimated to calculate the predicted AUC ($AUC_{PRED}$). The accuracy and precision of the $AUC_{PRED}$ values were assessed by calculating the mean prediction error (MPE) and root mean squared prediction error (RMSE), and compared with the target AUC of $5924{\mu}M{\cdot}min$. VPC showed that most data fell within the 95% prediction interval. MPE and RMSE of $AUC_{PRED}$ were -5.8% and 20.6%, respectively, in the conventional dosing group and -2.1% and 14.0%, respectively, in the new dosing scheme group. These findings demonstrated the validity of a new dosing scheme for daily intravenous busulfan used as conditioning therapy for HCT.

A study on performance-based evaluation system for NATM tunnels in use: development of evaluation model and validation (공용중인 NATM 터널의 성능중심 평가체계 연구: 평가모형 개발 및 검증)

  • Moon, Joon-Shik;Kim, Hong-Kyoon;An, Jai-Wook;Lee, Jong-Gun
    • Journal of Korean Tunnelling and Underground Space Association
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    • v.22 no.1
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    • pp.107-120
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    • 2020
  • In a performance-based evaluation of structures in use, the current performance is assessed by summing up the weighting of the evaluation indices for each performance. In this study, to suggest a performance-based evaluation technique for NATM tunnels in use, the performance evaluation indices were derived by examining the characteristics and similarities of each index developed from previous study. The weighting of the evaluation indices was derived by calculating the relative importance of each evaluation indices from the AHP analysis. In order to develop a quantitative evaluation model, grading criteria for each performance index was derived through literature review, and performance evaluation tables for road and railway tunnels were presented. In order to verify the significance of the proposed performance evaluation model, the correlation analysis was performed between each evaluation index and the final evaluation result. In the correlation analysis, the survey data measured through precision safety diagnosis in the tunnel in use was applied. It may be said that the proposed evaluation indices, weighting, criteria and evaluation models for tunnels in use can be applied to the performance-based maintenance system of tunnels.

Development of Dissolution Test for Itopride Hydrochloride Tablets and Tiropramide Hydrochloride Tablets (이토프리드염산염 정과 티로프라미드염산염 정의 용출시험법 개발)

  • Kim, Jung Hyun;Lee, Jong Hwa;Choi, Lan;Choi, Yeon Hee;Lee, Jong Chul;An, Ji Hye;Lee, Gwang Moon;Shim, Young Hoon;Kang, Shin-Jung;Sah, Hong-Kee;Choi, Hoo-Kyun;Kim, In-Kyu
    • YAKHAK HOEJI
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    • v.57 no.3
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    • pp.205-212
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    • 2013
  • Dissolution test has been performed to control drug quality and to predict in vivo drug release profile of solid dosage forms, so there's a drift towards setting dissolution test instead of disintegration test. However, some solid dosage forms in Korea Pharmaceutical Codex (KPC) are not established the dissolution test yet, so these monographs are necessary to set the specification of dissolution test. In this study, we developed the specification and test method of dissolution test for itopride hydrochloride tablets and tiropramide hydrochloride tablets which are not established the dissolution test yet. According to the "Manual for Guideline Application for Validation of Analytical Procedures" and "Guidelines on Specification of Dissolution test for Oral dosage form" of Korean Pharmacopoeia (KP), we validated and established each development method. Based on the preliminary dissolution profile, we set the dissolution condition(paddle apparatus, pH 1.2 media, 50 rpm). For this condition, we performed the main dissolution test to determine the specification (45 min, 85%). Finally, we validated each analytical method by specificity, linearity, accuracy and precision. These developed methods will be included the next supplement of KPC and also contributed to the quality control of medicines.

Rapid Determination of Ginsenosides Rb1, Rf, and Rg1 in Korean Ginseng Using HPLC (HPLC를 이용한 고려인삼 중 진세노사이드 Rb1, Rf 및 Rg1의 신속분석 방법 개발)

  • Hong, Hee-Do;Choi, Sang-Yoon;Kim, Young-Chan;Lee, Young-Chul;Cho, Chang-Won
    • Journal of Ginseng Research
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    • v.33 no.1
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    • pp.8-12
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    • 2009
  • A simple gradient HPLC method for rapid determination of major ginsenosides ($Rg_1$ and $Rb_1$) and unique ginsenoside (Rf) of Korean ginseng (Panax ginseng C.A. Meyer) was developed. Within 50min, three ginsenosides have been separated and identified on $\mu$-Bondapak $C_{18}$ column ($3.9{\times}300\;mm$, $10{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. The method was validated in terms of linearity, accuracy, and precision. The correlation coefficients ($r^2$) for calibration curves of ginsenosides were over 0.9997. The developed HPLC method was successfully applied to the analysis of ginseng samples and the recoveries of ginsenosides were in the range of $101.1{\sim}115%$ with RSD<3.2%. The developed method could be used for rapid evaluation of the ginsenosides $Rg_1$, $Rb_1$, and Rf.

Development and validation of an LC-MS/MS method for determination of compound K in human plasma and clinical application

  • Kim, Jung Soo;Kim, Yunjeong;Han, Song-Hee;Jeon, Ji-Young;Hwang, Minho;Im, Yong-Jin;Kim, Jung Hyun;Lee, Sun Young;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of Ginseng Research
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    • v.37 no.1
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    • pp.135-141
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    • 2013
  • A rapid, sensitive and selective analytical method was developed and validated for the determination of compound K, a major intestinal bacterial metabolite of ginsenosides in human plasma. Liquid-liquid extraction was used for sample preparation and analysis, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Compound K was analyzed on a Phenomenex Luna C18 column ($100{\times}2.00$ mm, 3 ${\mu}m$) with the mobile phase run isocratically with 10 mM ammonium acetate-methanol-acetonitrile (5:47.5:47.5, v/v/v) at a flow rate of 0.5 mL/min. The method was validated for accuracy (relative error <12.63%), precision (coefficient of variation <9.14%), linearity, and recovery. The assay was linear over the entire range of calibration standards i.e., a concentration range of 1 ng/mL to 1,000 ng/mL ($r^2$ >0.9968). The recoveries of compound K after liquid-liquid extraction at 1, 2, 400, and 800 ng/mL were $106.00{\pm}0.08%$, $103.50{\pm}0.19%$, $111.45{\pm}5.21%$, and $89.62{\pm}34.46%$ for intra-day and $85.40{\pm}0.08%$, $94.50{\pm}0.09%$, $112.50{\pm}5.21%$, and $95.87{\pm}34.46%$ for inter-day, respectively. The lower limit of quantification of the analytical method of compound K was 1 ng/mL in human plasma. The developed method was successfully applied to a pharmacokinetic study of compound K after oral administration in ten of healthy human subjects.

Development of Quantitative Analytical Method for Isoflavonoid Compounds from Fruits of Cudrania Tricuspidata (꾸지뽕나무 열매 isoflavonoid 화합물에 대한 정량분석법 개발)

  • Yoon, Sun Young;Kim, Seok Ju;Sim, Su Jin;Lee, Hak-Ju
    • Journal of the Korean Wood Science and Technology
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    • v.44 no.3
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    • pp.337-349
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    • 2016
  • In this study, an analytical method to evaluate the quality of isoflavonoid compounds purified and isolated from the fruits of Cudrania tricuspidata was developed and validated using Ultra Performance Liquid Chromatography (UPLC). The fruits of C. tricuspidata were extracted with methanol and further fractioned with n-hexane, ethyl acetate and water. The resulting ethyl acetate extract separated into four isoflavonoid compounds by a combination of silica gel and sephadex LH-20 column chromatography. The structures of the compounds were elucidated as alpinumisoflavone, 6,8-diprenyl genistein, 6,8-diprenyl orobol, 4'-O-methylalpinumisoflavone by various techniques such as UV-Vis, ESI-MS, $^1H\;NMR$ and $^{13}C\;NMR$ spectroscopy. Finally, a method to characterize the compounds was developed by using the UPLC equipped with a $C_{18}$ column and a gradient mobile phase system consisting of 2% acetic acid in water (solvent A) and 2% acetic acid in methanol (solvent B). The developed method was validated with the parameters such as selectivity, linearity, limit of detection, limit of quantitation, accuracy, and precision, which are defined by the ICH (International Conference on Harmonization). Using the validated method, the compounds in the fruits harvested in different months were also quantitatively analyzed. We propose this approach this approach can readily be utilized as an efficient evaluation method to quantify the extracts of C. tricuspidata.