• Mass Spectrometry Letters
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• 제13권3호
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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.

• 한국산업보건학회지
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• 제28권1호
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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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• 제40권1호
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• pp.1-11
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• 1997

• 기술사
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• 제17권4호
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• pp.56-61
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• 1984

• 농약과학회지
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• 제13권4호
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• pp.336-348
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• 2009

• 한국독성학회:학술대회논문집
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• 한국독성학회 2006년도 춘계학술대회
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• pp.90-92
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• 2006

• 한국환경보건학회:학술대회논문집
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• 한국환경보건학회 2001년도 춘계 학술대회
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• pp.101-102
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• 2001

• 방재기술
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• 통권6호
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• pp.37-42
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• 1989

• 상하수도학회지
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• 제27권6호
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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.

• 분석과학
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• 제35권3호
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• pp.93-115
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• 2022

의약품의 제조, 유통, 보관 과정에서 발생할 수 있는 잠재적 불순물은 의약품의 품질과 안전에 영향을 미치며 반응성이 높은 불순물의 경우 인체에 대한 발암성(변이원성)을 나타내기도 한다. 이를 위해 국제의약품규제조화위원회(International Conference on Harmonisation, ICH)에서는 "잠재적 발암 위해를 제한하기 위한 의약품 중 DNA 반응성(변이원성) 불순물의 평가 및 관리"에 대한 내용을 담은 M7(R1) 가이드라인을 제공하여 채택을 권고하였다. 하지만 가이드라인에서도 잠재적 불순물에 대한 분류, 섭취 허용량, 관리방안 등과 대표적인 불순물 14 종에 대한 가이드라인 적용을 소개하는데 그치고 있어 제약회사와 규제 당국에서 실제 관리를 위한 의약품 중 잠재적 불순물의 분석에 어려움을 겪고 있다. 이에 따라 본 총설에서는 비의도적 변이원성 불순물의 정의와 ICH M7(R1) 가이드라인에 소개된 내용을 간략하게 살펴보는 한편 현재까지 보고된 주요 잠재적 불순물의 분석 동향을 살펴보고자 한다. 이를 통해 식약처를 비롯한 감독 기관과 제약회사 등에서 의약품 중 잠재적 불순물 관리에 조금이나마 도움이 되고자 한다.