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研究生:陳盈絢
研究生(外文):Ying-Hsun Chen
論文名稱:以固相微萃取技術結合微波輔助建立尿中三鹵甲烷與鹵乙酸之同步分析方法
論文名稱(外文):Determination of Trihalomethanes and Halogenated Acetic Acids in Urine with Microwave-Assisted Solid-Phase Microextraction
指導教授:蔡詩偉蔡詩偉引用關係
指導教授(外文):Shih-Wei Tsai
學位類別:碩士
校院名稱:國立臺灣大學
系所名稱:環境衛生研究所
學門:醫藥衛生學門
學類:公共衛生學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:英文
論文頁數:58
中文關鍵詞:三鹵甲烷鹵乙酸微波輔助固相微萃取尿液
外文關鍵詞:THMsHAAsmicrowave assistedSPMEurine
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Trihalomethanes(THMs) and haloacetic acids(HAAs) are well known disinfection-by products (DBPs). DBPs can be formed by the reaction between the residual chlorine and the humic acids in raw water. People expose to DBPs through various daily activities, including swimming, for example. Due to poor ventilation and continuing adding organic matter from the swimmers, the concentrations of DBPs in swimming pools are usually higher than what was found in tap water.
The concentrations of DBPs in water as well as in air can be determined through environmental assessment. However, there are variations with human activities, rate of absorption, distribution, metabolism, and excretion. Therefore, it is difficult to assess the actual exposure through environmental monitoring. On the other hand, biological monitoring can be applied to evaluate the amounts human body absorbed, while blood, urine and expired breath were common specimens for biomonitoring. Among them, urine sample is favored because the procedure for sample taking is invasive, easily operated with convenience.
Current analytical method utilized different techniques to determine THMs and HAAs in urine, respectively. The procedures were cumbersome and time consuming. Therefore, the purpose of this study was to develop a co-analyzed method for THMs and HAAs in urin. The analytical procedure involved derivatization and extraction of THMs and HAAs simultaneously in urine with microwave assisted headspace solid phase microextraction(MAE-HS-SPME). Gas chromatography with electron capture detector (GC/ECD) was used for the determination. Parameters that might affect the derivatization and the extraction efficiency were optimized. The Carboxen/Polydimethylsiloxane (CAR/PDMS) fiber appeared to be most suitable for the analysis of THMs and HAAs. Besides, the efficiencies of the derivatization and extraction were increased by adding the same volume of acidic methanol as the sample for the derivatization. The esterification/extraction temperature was set at 45°C for 40 min with low stirring rate and without salt addition. For the desosrption and analysis, GC/ECD was used and the temperature of the injection port was set at 250°C and the SPME fiber was desorbed for 2 min. The matrix effect was observed in this study, hence the standard addition method is recommended to be applied. The relative standard deviations (RSDs) for the analysis were between 3.333%-24.052% and 3.615%-15.914% for THMs and HAAs, respectively. The accuracies were between 100±2.53% ~ 100±18.97% and 100±1.19% ~ 100±16.66% for THMs and HAAs, respectively. The method detection limits ranged from 0.043 to 30.33 ng/mL.
The effects of decomposition from trihaloacetic acids on the determination of THMs were also investigated.
致謝................................................ I
中文摘要.............................................II
ABSTRACT.............................................IV
TABLE OF CONTENTS....................................VI
LIST OF FIGURES ...................................VIII
LIST OF TABLES ......................................IX
CHAPTER 1 INTRODUCTION................................1
1.1 DISINFECTION BY-PRODUCTS IN WATER ................1
1.2 EXPOSURES OF DISINFECTION-BYPRODUCTS .............2
1.3 METABOLISM .......................................3
1.3.1 Trihalomethanes ................................3
1.3.2 Haloacetic acids ...............................3
1.4 HEALTH EFFECTS ...................................4
1.4.1 THMs ...........................................4
1.4.2 HAAs ...........................................5
1.5 BIOLOGICAL MONITORING.............................5
1.6 ANALYTICAL METHODS FOR THMs AND HAAs IN URINE.....7
1.7 OBJECTIVES........................................8
1.8 FRAMEWORK OF THE STUDY ...........................9
CHAPTER 2 MATERIALS and METHODS......................10
2.1 REAGENTS and MATERIALS ..........................10
2.2 METHODS .........................................12
2.2.1 Solid phase microextraction, SPME .............12
2.2.2. Microwave synthesis...........................14
2.3 EXPERIMENTAL ....................................15
2.3.1 Stock solutions and working solution ..........15
2.3.2 Urine treatment ...............................16
2.3.3 Sample derivatization and extraction procedure.16
2.3.4 Instrumentation ...............................17
2.3.5 Linearity, precision and recovery..............17
2.3.6 Matrix effects ................................17
CHAPTER 3 RESULTS AND DISCUSSIONS ...................18
3.1 FIBER SELECTION .................................18
3.2 DEORPTION TEMPERATURE and EFFICIENCY ............18
3.3 DERIVATIZATION –EXTRACTION TEMPERATURE..........19
3.4 DERIVATIZATION–EXTRACTION TIME..................19
3.5 DERIVATIZATIOG REAGENT...........................20
3.6 EFFECT OF IONIC STRENGTH.........................20
3.7 STIRRING RATE ...................................21
3.8 MATRIX EFFECT....................................21
3.9 METHOD VALIDATIONS ..............................21
3.10 THE DECOMPOSITION OF TRIHALOACETIC ACIDS .......23
CHAPTER 4 CONCLUSIONS ...............................24
REGERENCES...........................................26
APPENDIXES ..........................................31
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