全氟烷基化合物(perfluoroalkyl substances, PFASs) 具有抗油防水的特性，廣泛應用於工業製造及消費產品中，然而其持久性及毒性使其成為全球關注之環境汙染物。本研究為開發以超音波萃取搭配極致液相層析/串聯式質譜儀(ultra-performance liquid chromatography/tandem mass spectrometer, UPLC-MS/MS)對於20種PFASs多重殘留一次分析之方法，並實測七大類市售32件抗油食品包裝。本研究最適化UPLC-MS/MS各項參數，超音波萃取之最適合條件，並評估基質效應及萃取效率。最終依據食藥署規範，進行準確度(accuracy)及精密度(precision)之方法確效。100 cm2之樣品經裁剪成碎片後，以甲醇於50°C超音波萃取45分鐘，經離心、過濾、濃縮等步驟至1 mL，上機以UPLC-MS/MS分析。20種PFASs之基質效應因子(Matrix effect factors)為50.2%-80%，除PFHxDA, PFOSA, N-MeFOSA, 8:2 FTOH及8:2 diPAP低於50%；萃取效率(extraction efficiency)為51.5%-98.7%，除PFOSA, N-MeFOSA, 4:2 FTOH, 6:2 FTOH及8:2 FTOH低於6%。偵測極限(limits of detection, LODs)為0.07-11.3 ng/dm2；定量極限(limits of quantification, LOQs)為0.17-18.3 ng/dm2。方法確效(Method validation)參照食藥署公布之食品化學檢驗方法確效規範，20個待測物除4:2 FTOH之外，有19個PFASs通過準確度(accuracy)及精密度(precision)之要求，在三種不同濃度下，回收率(recovery)為70%-117%，精密度(%CV)低於19% (n = 5)，線性範圍為5.0-1,000 ng/dm2。實際檢測市售樣品，四件微波爆米花紙袋有三件可檢出短中碳鏈全氟羧酸(PFBA, PFPeA, PFHxA, PFOA, PFDA)，檢出範圍8.3-1,960 ng/dm2；兩件檢出氟調聚合醇類(FTOHs)，檢出範圍112-7,188 ng/dm2。三件通用防油紙袋有一件檢出全氟羧酸類(PFBA, PFHxA, PFOA, PFDA, PFUnDA, PFDoDA, PFHxDA)，檢出範圍5.7-48.6 ng/dm2；兩件檢出氟調聚合醇類(FTOHs)，檢出範圍454-2,595 ng/dm2。九件雞塊盒及薯條紙袋有兩件檢出全氟羧酸類(PFBA, PFHxDA)，檢出範圍5.0-40.3 ng/dm2；僅有一件檢出氟調聚合醇類(FTOHs)，檢出範圍22.4-167 ng/dm2。綜合言之，PFASs於各式抗油之食品包裝檢出濃度低至ppb等級，但仍須留意長期暴露的慢性健康影響。

Perfluoroalkyl substances (PFASs) possess oil-resistant and waterproof properties, and are widely used in industrial manufacturing and consumer products. Because of their persistency and toxicity, PFASs have become an environmental pollutant of global concern. A part of PFASs have been listed in the Stockholm Convention. The purpose of this study was to develop an analytical method for 20 PFASs with an ultra-performance liquid chromatography/triple-quadrupole tandem mass spectrometer (UPLC-MS/MS). This study also measured seven categories of commercial oil-resistant food packaging, in the total of 32 samples in Taiwan. This study optimized UPLC-MS/MS parameters, investigated suitable conditions for ultrasonic extraction, and evaluated the matrix effect and extraction efficiency. The finalized assay was validated according to the TFDA specification, to demonstrate good accuracy and precision. 100-cm2 samples were cut into pieces and were ultra-sonicated in 20-mL methanol at 50℃ for 45 minutes. The supernatant was centrifuged, filtered, and concentrated to 1 mL, then the residue was injected into UPLC-MS/MS. Matrix effect factors of 20 PFASs were 50.2%-80%, except for PFHxDA, PFOSA, N-MeFOSA, 8:2 FTOH and 8:2 diPAP were lower than 50%; extraction efficiencies were 51.5%-98.7%, except for PFOSA, N-MeFOSA, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH were lower than 6%. The linear dynamic ranges of the analytes were 5.0-1,000 ng/dm2 except for 4:2 FTOH didn’t comply with TFDA specifications. Most limits of detection (LODs) were between 0.07 and 11.3 ng/dm2; most limits of quantification (LOQs) were between 0.17 and 18.3 ng/dm2. The recoveries ranged from 70% to 117% on most analytes at three tested levels, and the precisions (%CV) were lower than 19% (n = 5). Three of four microwave popcorn packagings contained four- to nine-carbon perfluoroalkyl acids (PFBA, PFPeA, PFHxA, PFOA, PFDA) at 8.3-1,960 ng/dm2 and two of four contained FTOHs at 121-7,188 ng/dm2. One of three oil-proof paper bags contained perfluoroalkyl acids (PFBA, PFHxA, PFOA, PFDA, PFUnDA, PFDoDA, PFHxDA) at 5.7-48.6 ng/dm2; two of three were found FTOHs at 454-2,595 ng/dm2. PFBA and PFHxDA were observed at two of nine chicken boxes and fry paper bags, ranged from 5.0 to 40.3 ng/dm2; FTOHs were present in one of nine at 22.4-167 ng/dm2. PFASs were detected in some oil-resistant packaging. Although the concentrations of the observed levels on most samples were down to ppb levels, long-term exposure to them chronic adverse health effects from warrants further attention.

口試委員會審定書 #
誌謝 i
中文摘要 ii
ABSTRACT iii
CONTENTS v
LIST OF FIGURES vii
LIST OF TABLES viii
Chapter 1 Introduction 1
1.1 Perfluoroalkyl substances (PFASs) 1
1.2 Determination of oil-resistant food packagings 4
1.3 Objectives 7
Chapter 2 Methods 9
2.1 Reagents and materials 9
2.2 Instruments 10
2.3 Sample collection 11
2.4 Sample preparation 11
2.5 Instrumental analysis 12
2.5.1 Optimization of MS/MS parameters for analytes 12
2.5.2 Optimization of UPLC-MS/MS analytical conditions 13
2.6 Method validation 14
2.6.1 Matrix effect and extraction efficiency 14
2.6.2 Assessment of accuracy and precision 15
2.6.3 Identification, quantification, and data analysis 15
2.6.4 Quality assurance and quality control 16
Chapter 3 Results and Discussions 17
3.1 MS/MS parameter 17
3.2 Chromatography 17
3.2.1 Selection of columns and mobile phases 17
3.2.2 Adjustment of UPLC gradient 19
3.3 Sample preparation 20
3.3.1 Temperature stability test of ultrasonic extraction 20
3.3.2 Optimization of ultrasonic extraction 21
3.3.3 Comparison of static extraction and ultrasonic or volatilization extraction 22
3.3.4 Matrix effect test 23
3.3.5 Adjustment of concentration processes 24
3.4 Method validation 25
3.4.1 IDLs, IQLs, and calibration range 25
3.4.2 LODs and LOQs 26
3.4.3 Matrix effect and extraction efficiency 27
3.4.4 Accuracy and precision 28
3.4.5 Matrix transfer factor 30
3.5 Real sample 32
Chapter 4 Conclusions 37
Reference 39
Figures 45
Tables 60

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