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Development of an Optimized Target Analysis Method for Monitoring PPCPs in Drinking and Raw Water in Korea

  • 나태호 (서강대학교 일반대학원)

초록 (요약문)

Pharmaceuticals and personal care products (PPCPs) enter the environment through pesticides, hygiene products, detergents, and pharmaceuticals, and negatively impact water quality due to their resistance to biodegradation. These substances are challenging to identify in aquatic environments due to their diverse polarities and the lack of optimized analytical techniques, necessitating highly sensitive methods for accurate analysis. This research optimized an efficient analytical method for detecting 17 PPCPs suspected to be present in drinking and raw waters in Korea, using solid-phase extraction, liquid chromatography, and Orbitrap mass spectrometry. The optimization process included adjustments to mass spectrometry, extraction cartridges, and extraction pH conditions to minimize matrix effects and achieve high recoveries. Sensitivity in mass spectrometry was enhanced by comparing CID and HCD modes, and a tandem solid-phase extraction technique was developed by combining a hydrophilic-lipophilic balance (HLB) cartridge with a weak cation exchange (WCX) cartridge after testing various cartridges and pH conditions. The detection limit of the optimized method ranged from 0.001 to 0.05 μg/L, demonstrating excellent performance with linearity above 0.99, accuracy between 75.18% and 123.42%, and precision from 2.04% to 21.94%. Extraction efficiency was evaluated in purified water, yielding recoveries of 38.19% to 129.36% for analytes with a wide range of polarities (Log Pow -1.8 to 5.27). The optimized analytical method developed in this study enhances precision and sensitivity, providing a robust foundation for monitoring PPCPs in treated and raw water in South Korea.

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초록 (요약문)

제약 및 개인위생 관리제품(PPCPs)은 살충제, 위생제품, 세척제 및 의약품을 통해 환경으로 유입되며, 자연분해에 강해 수질에 부정적인 영향을 미칩니다. 이들 물질은 다양한 극성으로 인해 최적화된 분석기술이 부족하여 수생환경에서 식별이 어려우므로, 정확한 분석을 위한 고감도 기법이 요구됩니다. 본 연구에서는 고체상추출, 액체크로마토그래피, 오비트랩 질량분석기를 활용하여 우리나라 정수 및 원수에서 검출 가능성이 있는 17가지 PPCPs의 효율적인 분석 방법을 최적화하였습니다. 방법 최적화 과정에서는 매트릭스 효과를 최소화하고 높은 회수율을 확보하기 위해 질량분석과 추출카트리지, 추출 pH 조건을 최적화하였습니다. 질량분석에서는 CID와 HCD모드 비교를 통해 감도를 향상시켰으며, 다양한 카트리지와 pH 조건을 실험하여 친수성-친유성 밸런스 카트리지(HLB)와 약한 양이온 교환카트리지(WCX)를 결합한 텐덤 고체상추출 기술을 개발하였습니다. 최적화된 분석 방법의 검출한계는 0.001 - 0.05 μg/L 범위였으며, 선형성 0.99 이상, 정확도 75.18 - 123.42%, 정밀도 2.04% - 21.94%로 우수한 성능을 보였습니다. 추출효율은 정제수에서 평가되었으며, 광범위한 극성(LogPow –1.8 – 5.27)을 지닌 분석물질의 회수율은 38.19 % - 129.36 % 였습니다. 본 연구에서 최적화된 분석법은 정밀성과 민감도를 향상시켜 한국의 정수 및 원수 내 PPCPs 모니터링에 중요한 기반을 제공할 것으로 기대됩니다.

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목차

1. Introduction 1
2. Materials and Methods 6
2.1. Chemicals and reagents 6
2.2. Sample pretreatment and solid-phase extraction 9
2.3. UHPLC-HRMS/MS 11
2.4. Quality assurance and method validation 12
3. Result and Discussion 13
3.1. Optimization of mass spectrometry for target analytes 13
3.1.1. Comparison of CID and HCD mass spectrum 13
3.1.2. Selection of optimal collision mode based on SY values 15
3.2. Optimization of recovery rates for highly polar analytes 21
3.2.1. Performance assessment of the Oasis HLB cartridge 21
3.2.2. Performance assessment of Ion Exchange cartridges under varied pH conditions 24
3.2.3. Tandem HLB-WCX extraction method 30
3.3. Quality assurance and method validation 32
4. Conclusion 36
Reference 38

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