• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.17 no.4
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• pp.363-373
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• 2019

Waste characterisation associated with nuclear site decommissioning relies on radiochemical analysis of a diverse range of sample types, requiring extensive validation of analytical techniques using matrix-matched materials. The absence of relevant reference materials has hindered robust method development and validation. The paper discusses how method validation in support of nuclear waste characterisation can be achieved without using reference materials. The key stages in an analytical procedure are evaluated and a multi-stage approach is proposed with the ultimate aim of determining an operational envelope for an analytical procedure.

• Analytical Science and Technology
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• v.37 no.2
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• pp.114-122
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• 2024

A transmission Raman spectroscopy-based quantitative model, which can analyze the content of a drug product containing naproxen sodium as its active pharmaceutical ingredient (API), was developed. Compared with the existing analytical method, i.e., high-performance liquid chromatography (HPLC), Raman spectroscopy exhibits high test efficiency owing to its shorter sample pre-treatment and measurement time. Raman spectroscopy is environmentally friendly since samples can be tested rapidly via a nondestructive method without sample preparation using solvent. Through this analysis method, rapid on-site analysis was possible and it could prevent the production of defective tablets with potency problems. The developed method was applied to the assays of the naproxen sodium of coated tablets that were manufactured in commercial scale and the content of naproxen sodium was accurately predicted by Raman spectroscopy and compared with the reference analytical method such as HPLC. The method validation of the new approach was also performed. Further, the specificity, linearity, accuracy, precision, and robustness tests were conducted, and all the results were within the criteria. The standard error of cross-validation and standard error of prediction values were determined as 0.949 % and 0.724 %, respectively.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.19 no.2
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• pp.96-101
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• 2009

The purpose of this study was to conduct the field validation of alternative method(ETM method) by using non-carcinogenic, and less toxic solvents than NIOSH (National Institute for Occupational Safety and Health) analytical method 5524 for measuring the airborne metalworking fluids in workplaces. We carried out the field validation test by using the exposure chamber, guaranteeing the air sampling homogeneously in a machining environment. The ETM mixed solvent presented the complete solubility of MWFs used in test field. Based on the field test data, the bias of the ETM method from reference method, NIOSH analytical method 5524, was from -7.0% to 5.1%. The overall uncertainty of the ETM nethod was 21.6%, which satisfied the NIOSH criteria for the sampling and analytical criteria.

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

• Korean Journal of Pharmacognosy
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• v.38 no.1
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• pp.19-21
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• 2007

Myristica fragrans has been used for the treatment of stomachache in East Asia. It is very important to determine the amount of myristicin in Myristica fragrans, because excess myristicin causes side effects. In this study, we developed and validated the method for determination contents of myristicin in Myristica fragrans which was purchased from various regions of Korea. The average content of myristicin in Myristica fragrans was 2.10% with the validated HPLC analysis method.

• Analytical Science and Technology
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• v.37 no.3
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• pp.131-142
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• 2024

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

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

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