• Journal of Korean Society for Quality Management
• /
• v.50 no.4
• /
• pp.831-842
• /
• 2022

Purpose: This study carried out the Quality by Design (QbD)6σ process to verify the effectiveness and equivalence of the finished D-antigen quantitative test method, and compared the OFAT-based method validation and test result acceptance criteria with the Analytical Quality by Design (AQbD)-based method validation and test method. This is a study on how to reduce the risk of delay in permit change by increasing the reliability of permit data in the existing method by statistically analyzing the results. Methods: With the QbD6σ process, the effectiveness and equivalence of the D-antigen quantitative test method were verified with the data of the existing test method and the new test method. Results: Method validation tests are performed based on AQbD. Critical Method Parameters are identified through risk assessment, and single/combined actions are verified by designing and performing tests for Critical Method Parameters (analysis of variance, full factorial design method). Method validation can be effectively accomplished with the QbD6σ process. Conclusion: The use of QbD6σ can be used to achieve satisfactory results for both pharmaceutical companies and regulators by using appropriate statistical analytical methods for method validation as required by regulatory agencies.

• Spatial Information Research
• /
• v.21 no.2
• /
• pp.45-54
• /
• 2013

Analytical and simulation error models have the ability to describe (or realize) error-corrupted versions of spatial data. But the different approaches for modeling positional errors require an internal validation that ascertains whether the analytical and simulation error models predict correct positional errors in a defined set of conditions. This paper presents stochastic simulation models of a point and a line segm ent to be validated w ith analytical error models, which are an error ellipse and an error band model, respectively. The simulation error models populate positional errors by the Monte Carlo simulation, according to an assumed error distribution prescribed by given parameters of a variance-covariance matrix. In the validation process, a set of positional errors by the simulation models is compared to a theoretical description by the analytical error models. Results show that the proposed simulation models realize positional uncertainties of the same spatial data according to a defined level of positional quality.

• Analytical Science and Technology
• /
• v.32 no.3
• /
• pp.88-95
• /
• 2019

This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

• Analytical Science and Technology
• /
• v.35 no.2
• /
• pp.60-68
• /
• 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.

• Proceedings of the Korean Society of Applied Pharmacology
• /
• 2002.07a
• /
• pp.158-169
• /
• 2002

본 발표에서는 약물 분석 중 특히 생체 매질을 이용하여 임상약리학적 연구나 생체 내 이용률(bioavailability) 연구, 생물학적 동등성(bioequivalence) 연구를 하는 경우의 분석법 검증(bioanalytical method validation)에 대하여 상세히 설명하고자 한다.

• Journal of Environmental Health Sciences
• /
• v.41 no.5
• /
• pp.358-367
• /
• 2015

Objectives: This study was performed to evaluate the analytical method for PAH metabolites in human urine using enzyme hydrolysis and solid-phase extraction coupled with LC-(ESI)-MS/MS technique. Methods: We employed HPLC tandem mass spectrometry techniques with appropriate pre-treatment for analysis of 16 OH-PAHs in human urine. Samples were hydrolysis by ${\beta}$-flucuronidase/Aryl sulfatase, and target compounds were extracted by solid-phase extraction with a strata-x cartridge. Cross-validation was performed between Eulji University and Green Cross laboratories with 200 human urine samples. Results: The accuracies were between 90.3% and 118.8%, and precisions (relative standard deviations) were lower than 10%. The linearity obtained was satisfying for the 16 OH-PAH compounds, with a coefficient of determination ($r^2$) higher than 0.99. The results of cross-validation at the two organizations were compared by ICC (interclass correlation coefficient) values. The cross-validation results were excellent or good for all compounds. Conclusion: An analytical method was validated for low nanogram levels of 16 OH-PAHs in human urine. Also, satisfying results were obtained for method validation such as accuracy, precision and ICC of cross-validation.

• Analytical Science and Technology
• /
• v.28 no.3
• /
• pp.160-167
• /
• 2015

This study aims to develop a new analytical method to detect zinc pyrithione, the ingredient of cosmetics appointed as restricted ingredients and used as preservatives.. The analytical method was based on data gathered from the relevant literature. Information about the amounts of these ingredients was researched in order to select the base-matrix materials used to validate the analytical method. After selecting and preparing the base-matrix materials, the analytical method was validated by method validation procedures. The analytical method was verified first by inter-laboratory validation and then through analyzing the cosmetics sold in the market. Based on the results of this study, guidelines are proposed for the analysis of restricted ingredients in cosmetics, which will provide a method to test the cosmetics circulating in the Korean market. The use of the proposed guidelines will increase the quality of the cosmetics as well as the safety of human health, which will enhance the competitiveness of the Korean cosmetics industry and lead to an increase in the exportation of cosmetics.

• Proceedings of the PSK Conference
• /
• 2004.10a
• /
• pp.140-140
• /
• 2004

• Analytical Science and Technology
• /
• v.32 no.4
• /
• pp.139-146
• /
• 2019

A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.

• Journal of Digestive Cancer Research
• /
• v.11 no.3
• /
• pp.157-164
• /
• 2023

Prediction is a significant topic in clinical research. The development and validation of a prediction model has been increasingly published in clinical research. In this review, we investigated analytical methods and validation schemes for a clinical prediction model used in digestive cancer research. Deep learning and logistic regression, with split-sample validation as an internal or external validation, were the most commonly used methods. Furthermore, we briefly introduced and summarized the advantages and disadvantages of each method. Finally, we discussed several points to consider when conducting prediction model studies.