• Mass Spectrometry Letters
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• v.13 no.3
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• pp.58-83
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• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.28 no.1
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• pp.108-116
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• 2018

Objectives: This study investigated to the analytical work environment, analyst's expert and status of analytical instrument in the designated organization's laboratory for measuring work environment, and carried out to ensure reliability of analytical results. Methods: This study was conducted by 114 analysts who work in designated organization's laboratory for measuring work environment. Information on the working environment and personal characteristics of the analysts were collected using a self-reported questionnaire and were analyzed using the SPSS program through analysis of frequency and t-test. Results: The speciality of subjects was occupational health(57.0%), environmental health(38.6%) and environmental engineering(4.4%), and they had a higher level of academic ability than workers in other industries. Analysts had to handle a large number of sample analysis and many tasks other than analytical work. The analysts answered that it was difficult to analyze organic substances than inorganic substances, and the difficult parts were the analytical methods setting of new substances(55.3%), instrument analysis(24.6%) and principle of analysis(23.7%). Analytical instruments mainly have legally required instruments. The difficulty of the analysis is solved from the senior analyst in the laboratory and analytical information is mainly exchanged through seminar organized by the Association of Occupational Health Analysts. The analysts who are planning to move or considering the company were 48.2%, and the reasons for moving the company were difficult to work(14.0%), low salary(9.6%), employment type(8.8%) and job stress(7.0%). Conclusions: The conclusions of our study were that it was possible to secure reliability by solving the problems such as implementing professional education to improve expertise of analysts, strengthening analytical instruments through institutional improvement and improving work environment.

• Applied Biological Chemistry
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• v.40 no.1
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• pp.1-11
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• 1997

• Journal of the Korean Professional Engineers Association
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• v.17 no.4
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• pp.56-61
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• 1984

• The Korean Journal of Pesticide Science
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• v.13 no.4
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• pp.336-348
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• 2009

• Proceedings of the Korean Society of Toxicology Conference
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• 2006.05a
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• pp.90-92
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• 2006

• Proceedings of the Korean Environmental Health Society Conference
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• 2001.04a
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• pp.101-102
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• 2001

• Fire Protection Technology
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• s.6
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• pp.37-42
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• 1989

• Journal of Korean Society of Water and Wastewater
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• v.27 no.6
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• pp.827-836
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• 2013

Due to the stringent drinking water quality, formaldehyde will be included in Korean drinking water standard from year 2014. However, its standard analytical method has not yet been established. This study compares two analytical methods, DNPH-LC and ACFAS with respect to their analysis principles, Method Detection Limit (MDL), Limit Of Quantitation(LOQ), precision, accuracy, reproducibility, convenience, number of samples analyzed per hour and analysis cost. These methods measure absorption intensity at 360 nm by using HPLC after DNPH-derivatization (DNPH-LC) and at 410 nm by using Automated Continuous Flow Absorption Spectrophotometer (ACFAS), respectively. Reproducibility was tested by repeating the analysis 7 times using a standard solution for each method. For DNPH-LC method, MDL was $0.5{\mu}g/L$, LOQ was $1.58{\mu}g/L$ with standard deviation of $0.16{\mu}g/L$. For ACFAS method, they were $0.27{\mu}g/L$, $0.85{\mu}g/L$L with standard deviation of $0.09{\mu}g/L$, respectively. Both methods satisfied the requirement set by the Korean drinking water quality standard. Complexity of sample pretreatment procedure for DNPH-LC method may cause large error and, consequently, the analytical result will depend on the level of skill of analyst. In contrast, ACFAS method which used only one reagent equipped with an automated injection device showed little analytical error. It costs about $5.00 and $1.00 for one sample to analyze by the DNPH-LC method and the ACFAS method, respectively. Compared to the DNPH-LC method, ACFAS method provided more reliable analytical results. In terms of convenience, easiness and analytical cost, ACFAS method was demonstrated to be superior to the DNPH-LC method. The results of this study suggested that the ACFAS method could be adapted as a proper method for determining formaldehyde content in drinking water.

• Analytical Science and Technology
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• v.35 no.3
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• pp.93-115
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• 2022

Potential impurities in pharmaceuticals could be produced during manufacture, distribution, and storage and affect quality and safety of pharmaceuticals. In particular, highly reactive impurities could result in carcinogenic (mutagenic) effects on human body. International Conference on Harmonisation (ICH) has provided M7(R1) guideline for "Assessment and Control of DNA Reactive (Mutagenic) Impurities in Pharmaceuticals to Limit Potential Carcinogenic Risk" and recommended an adoption of this guideline to the authorities. ICH M7(R1) guideline provides classification, accepted intakes, and controls of potential impurities in pharmaceuticals. However, since appropriate and unified analytical methods for impurities in pharmaceuticals have not been provided in this guideline, most potential impurities in pharmaceuticals are still difficult to manage and supervise by pharmaceutical companies and regulatory authorities, respectively. In this review, we briefly described definition of unintended mutagenic impurities, basic information in ICH M7(R1) guideline, and analytical methods to determine potential impurities. This review would be helpful to manage and supervise potential impurities in pharmaceuticals by pharmaceutical companies and regulatory authorities.