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GC-MS를 이용한 일회용 생리대 중 프탈레이트 및 비스페놀 A의 동시분석법 개발 및 검증

Development and validation of GC-MS method for simultaneous determination of phthalate esters and bisphenol A in disposable sanitary products

초록/요약

Disposable sanitary products (DSPs) are made up of various raw materials including natural/synthetic polymers and adhesives. Phthalate esters (PAEs) are the platicizers used in synthetic polymers such as polystyrene. Because PAEs may be intentionally or unintentionally contained in DSPs from the raw materials or manufacturing processes, there has been growing concerns over the exposure to PAEs from the use of DSPs. In this study, we aimed to develop and validate GC-MS method for simultaneous determination of 15 regulated phthalates and bisphenol A in DSPs. Analytical method was developed through optimization of sample preparation using ultrasonic extraction and GC-MS analytical conditions. Developed analytical method was validated following the ICH guideline in terms of specificity, linearity, LOQ, precision, and accuracy. All of method validation parameters satisfied acceptance criteria, suggesting that this method was suitable and reliable for monitoring the target analytes in DSPs. When this method is applied to the commercial DSPs (N=106), 5 PAEs were found and determined. Our simple and reliable method will be useful as the quality control of PAEs levels in DSPs and further contribute to resolve safety issue as an analytical tool for risk assessment of PAEs exposure from the use of DSPs.

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목차

1. Introduction 1
1.1 Phthalate esters (PAEs) 1
1.1.1 Characteristic and application 1
1.1.2 Human exposure 2
1.1.3 Toxicities 3
1.1.4 Regulation 4
1.2 Disposable sanitary products (DSP) 5
1.3 Analytical methods for PAEs in diverse matrices 6
1.4 Aims of this study 7
2. Experimental 10
2.1 Chemicals, reagents, and instrument 10
2.1.1 Chemicals 10
2.1.2 Reagents and equipment 11
2.2 Samples 12
2.3 Preparation of solution 12
2.3.1 Standard mix solution 12
2.3.2 Internal standard and surrogate solution 12
2.4 Method development 13
2.4.1 Analytical column 13
2.4.2 Extraction solvent 13
2.4.3 Extraction time 14
2.5 Standard and sample solution preparation 14
2.5.1 Preparation of matrix-matched standard solution 14
2.5.2 Preparation of sample solution 16
2.5.3 GC-MS conditions 16
2.6 Validation 19
2.6.1 Specificity 19
2.6.2 Linearity 19
2.6.3 Limit of detection (LOD) and limit of quantitation (LOQ) 19
2.6.4 Accuracy and precision 20
3. Result and discussion 21
3.1 Method development 21
3.1.1 Oven temperature and column 21
3.1.2 Extraction solvent optimization 23
3.1.3 Ultrasonic extraction time optimization 25
3.2 Validation results 27
3.2.1 Specificity 27
3.2.2 Linearity 29
3.2.3 Accuracy and Precision 31
3.3 Sample Extraction Results 34
4. Conclusion 37
5.References 38

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