• Natural Product Sciences
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• v.10 no.6
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• pp.262-267
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• 2004

A reversed-phase liquid chromatographic method for decursin and decursinol angelate of Angelicae gigantis Radix, an important crude drug in Korean traditional medicine, was developed and validated. Decursin and decursinol angelate, the structure isomer (pyranocoumarin) each other, are the main organic constituents in Angelicae gigantis Radix. This method was developed using a RP-18 column, UV detector at 280 nm and 50% acetonitrile solution containing 0.01 M sodium dodecyl sulfate and 25 mM sodium dihydrogen phosphate (pH 5.0) as the mobile phase. Various validation parameters were included and evaluated satisfactorily. Linearity was established in range 2-75 mg/ml of decursin and decursinol angelate (correlation coefficient = 0.9997 and 0.9995, respectively). This analytical method showed good accuracy (98.1% and 99.5%, respectively). Precision (repeatability) revealed a relative standard deviation value of 1.71% (decursin) and 3.19% (decursinol angelate). For intermediate precision measure the considered variables were equipment and days. A robustness test showing the influence of deferent counter-ion concentration in mobile phase was also performed.

• Journal of Internet Computing and Services
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• v.17 no.5
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• pp.131-139
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• 2016

This paper presents a workflow validation method for data-intensive graphical workflow models using real-time workflow tracing mode on data-intensive workflow designer. In order to model and validate workflows, we try to divide as modes have editable mode and tracing mode on data-intensive workflow designer. We could design data-intensive workflow using drag and drop in editable-mode, otherwise we could not design but view and trace workflow model in tracing mode. We would like to focus on tracing-mode for workflow validation, and describe how to use workflow tracing on data-intensive workflow model designer. Especially, it is support data centered operation about control logics and exchange variables on workflow runtime for workflow tracing.

• Korean Journal of Food Science and Technology
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• v.53 no.6
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• pp.682-687
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• 2021

The purpose of this study was to validate a high-performance liquid chromatography (HPLC) method for the quantitative analysis of quercetin in various foods. The method was based on HPLC-UV (360 nm). The method was validated using candy, beverage, and sausage which were tested for specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy, and the measurement uncertainty was assessed. Matrix-matched calibration was also applied. The calibration curves (0.5-50 mg/L) showed good linearity (r²≥0.9998). LOD and LOQ ranged from 0.15 to 0.31 mg/kg and from 0.44 to 0.93 mg/kg, respectively. The average accuracy and precision at 0.5, 2.5, and 10 mg/kg ranged from 84.3 to 102.0% and 0.7 to 3.0 relative standard deviation (RSD%), respectively. This study confirmed the applicability of the proposed method by applying it to commercial products, such as teas and beverages. Thus, the proposed analytical method is suitable for quantifying quercetin in various foods.

• Korean Journal of Pharmacognosy
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• v.41 no.1
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• pp.48-53
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• 2010

GCSB-5 preparation is a purified extract from a mixture of 6 medicinal plants(Acanthopanacis Cortex, Achyranthis Radix, Saposhnikoviae Radix, Cibotii Rhizoma, Glycine Semen Nigra, Eucommiae Cortex) that have been widely used for the treatment of various bone disorders. The aim of this study was to investigate HPLC analysis method and screening of standard compound on Cibotii Rhizoma for quality standardization of a medicinal crude drug GCSB-5. Onitin-4-O-$\beta$-D-glucopyranoside was isolated from Cibotii Rhizoma as the standard compound and identified on the basis of spectroscopic data such as NMR. HPLC analysis method for the determination of onitin-4-O-$\beta$-D-glucopyranoside was established for the quality control of the medicinal plants of Cibotii Rhizoma species, GCSB-5 raw material and GCSB-5 preparation. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline.

• YAKHAK HOEJI
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• v.52 no.2
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• pp.93-100
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• 2008

A liquid chromatographic method with tandom spectrometric detection (LC/MS/MS) for the simultaneous determination of doxifluridine and its active metabolite, 5-fluorouracil (5-FU) was developed over the concentration range of $5{\sim}2000$ ng/ml, respectively. Doxifluridine, 5-FU and internal standard, 5-chlorouracil (5-CU), were extracted from liver and intestine tissue via protein precipitation. Acetonitrile was used as the extraction solvent and the supernatant was evaporated and reconstructed in mobile phase. Optimum chromatographic separation was achieved on a Agilent Zorbax $C_{18}$ ($100\;mm{\times}2.1\;mm$, $3.5\;{\mu}m$) column with mobile phase run in isocratic with methanol : water (20 : 80, v/v). The flow rate was 0.2 ml/min with total cycle time of 5 min. The lower limit of quantification was validated at 5.0 ng/ml of liver and intestine tissue, for both doxifluridine and 5-FU, respectively. The intra-day and inter-day precision and accuracy of quality control (QC) samples were <11% coefficient of variation and <7% relative error from theoretical concentration for both analytes. In addition, the special designed stability study was performed, because the metabolism of doxifluridine occurs spontaneously even in ice bath for monkey liver. The stability of doxifluridine in liver and intestine of monkey and beagle dog was compared. It was found that bioanalytical validation could not be performed for the monkey liver; however, beagle dog's liver has relatively low speed of metabolism compared to monkey liver and instead of monkey liver, beagle dog's liver could be used for the validation. Bioanalytical validation could be performed in monkey intestine. Eventually, this developed method for liver and intestine will be useful in support of the toxicokinetic and pharmacokinetic studies of doxifluridine and 5-FU.

• Food Science of Animal Resources
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• v.43 no.6
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• pp.949-960
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• 2023

This research aimed to validate a high-performance liquid chromatography method for the quantitative determination of bixin and norbixin in various foods. The Diode Array Detector (495 nm) technique was used. Method was validated for specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy, and the measurement uncertainty was assessed. The calibration curve showed excellent linearity (r²≥0.9999) over the tested concentration range of 0.2-25 mg/L. The LOD and LOQ were 0.03-0.11 and 0.02-0.05 mg/L for bixin and norbixin, respectively. The intra-and inter-day accuracies and precisions were 88.0±1.3-97.0±0.5% and 0.2%-2.6% relative SD (RSD) for bixin and 88.2±0.8-105.8±0.8% and 0.3%-2.7% RSD for norbixin, respectively. Inter-laboratory validation for accuracy and precision was conducted in three laboratories, and these results all met the AOAC guidelines. In addition, the relative expanded uncertainty (<22%) satisfied the CODEX recommendation. Furthermore, products distributed in Korea were monitored for annatto extracts using the proposed method to demonstrate its application. The developed analytical method is reliable for quantifying bixin and norbixin in various foods.

• Fisheries and Aquatic Sciences
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• v.23 no.3
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• pp.9.1-9.6
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• 2020

Background: Fucosterol is a compound commonly found in algae that has various biological activities. The purpose of this study was to develop a high-performance liquid chromatography (HPLC) validation method for fucosterol and to compare the fucosterol contents of 11 algal species from Ulleungdo, Korea. Method: In this study, we successfully isolated and identified fucosterol from a 70% EtOH extract of Sargassum miyabei, and subsequently conducted specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision analyses for development of an HPLC validation method. Fucosterol contents were compared using the established HPLC validation conditions. Results: We successfully isolated fucosterol from a 70% EtOH extract of S. miyabei and identified it based on spectroscopic analysis. On the basis of HPLC validation using the fucosterol isolated from S. miyabei, we confirmed specificity (8.5 min), linearity (R² = 0.9998), LOD (3.20 ㎍ mL^-1), LOQ (9.77 ㎍ mL^-1), accuracy (intra-day and inter-day variation, 90-110%), and precision (RSD, 1.07%). Fucosterol contents in the 11 assessed algal species ranged from 0.22 to 81.67 mg g^-1, with the highest content being recorded in a 70% EtOH extract of Desmarestia tabacoides (81.67 mg g^-1), followed by that of Agarum clathratum (78.70 mg g^-1). Conclusions: The results indicate that 70% EtOH extracts of D. tabacoides and A. clathratum containing fucosterol with various effects can be potential alternative sources of fucosterol.

• Journal of Pharmacopuncture
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• v.12 no.4
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• pp.33-50
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• 2009

Objectives : This study was conducted to confirm validation and stability of concentration analysis method of pure melittin (Sweet Bee Venom-Sweet BV) extracted from the bee venom by utilizing protein isolation method of gel filtration. Methods : All experiments were conducted at Biotoxtech, a non-clinical studies authorized institution, under the regulations of Good Laboratory Practice (GLP). Standard solutions of melittin (SIGMA, USA) and test substances were dispensed and were analyzed with HPLC for Sweet BV to secure the validation of analysis. Results : 1. Measurement of system suitability of Sweet BV satisfied criterion of below 3%. 2. Confirming Linearity of Sweet BV in 10-200${\mu}g/m\ell$ solution yielded correlation coefficient (r) of 0.995 and accuracy of 85-115% which satisfy criterion. 3. Measurement of Specificity of Sweet BV didn't yield any substance affecting the peak of test substances, but detected at 21.22min verified as the test substance. 4. Confirming Intra-day of Sweet BV, accuracy and precision of 0.1, 100${\mu}g/m\ell$ were 105.70, 95.81 and 0.66, 0.73, respectively, satisfying both criteria of accuracy (85-115%) and precision (within 10%). 5. To measure Stability in autosampler, all samples used in Intra-day reproducibility sat in the autosampler for five hours and were re-analyzed. Both variability and precision satisfied the criteria. 6. Homogeneity of Sweet BV (0.1, 100${\mu}g/m\ell$) at upper, middle, and lower layers all satisfied the accuracy and precision criteria. 7. Stability of Sweet BV (0.1, 100${\mu}g/m\ell$) at room temperature for four hours and refrigerated for 7 days all satisfied the criterion. 8. For the measurement of Quality control, QC samples measured on the first and eighth day all satisfied accuracy and precision criteria. Conclusion : Above experiment data satisfies validation and stability of concentration analysis method of Sweet BV.

• Journal of the Korean Data and Information Science Society
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• v.22 no.5
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• pp.999-1005
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• 2011

This paper proposes a weighted least squares support vector machine for asymmetric least squares regression. This method achieves nonlinear prediction power, while making no assumption on the underlying probability distributions. The cross validation function is introduced to choose optimal hyperparameters in the procedure. Experimental results are then presented which indicate the performance of the proposed model.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.11
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• pp.1682-1686
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• 2015

This study was conducted to establish an HPLC analysis method for determination of marker compounds as part of materials standardization for development of health functional food materials from pear pomace. The quantitative determination method of caffeic acid and chlorogenic acid as marker compounds of pear pomace extract (PPE) was optimized by HPLC analysis using a C18 column ($5{\times}250mm$, $5{\mu}m$) with a 0.2% elution gradient of acetic acid and methanol as the mobile phase at a flow rate of 0.8 mL/min and detection wavelength of 330 nm. The HPLC/UV method was applied successfully to the quantification of marker compounds in PPE after validation of the method with linearity, accuracy, and precision. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999, and limit of detection and limit of quantification were $1.14{\mu}g/mL$ (caffeic acid) and $1.61{\mu}g/mL$ (chlorogenic acid) as well as $4.9{\mu}g/mL$ (caffeic acid) and $4.9{\mu}g/mL$ (chlorogenic acid), respectively. Relative standard deviation values from intra- and inter-day precision were less than 3.1% (caffeic acid) and 4.0% (chlorogenic acid), respectively. Recovery rates of caffeic acid and chlorogenic acid at 12.5, 25, and $50{\mu}g/mL$ were 93.66~106.32% and 97.33~105.68%, respectively. An optimized method for extraction of caffeic acid and chlorogenic acid in PPE was established through diverse extraction conditions, and the validation indicated that the method is very useful for evaluation of marker compounds in PPE to develop a health functional food material.