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研究生:溫莎拉
研究生(外文):Sarawinda Hutagalung
論文名稱:QuEChERS結合液相層析串聯質譜於蔬菜中之清潔劑檢測
論文名稱(外文):Determination of Surfactants in Vegetable by Using QuECHERS Combined with LC-MS/MS
指導教授:李茂榮李茂榮引用關係
指導教授(外文):Maw-Rong Lee
口試委員:楊慶成鄭政峰
口試委員(外文):Thomas C YangJen-Fon Zen
口試日期:2016-07-07
學位類別:碩士
校院名稱:國立中興大學
系所名稱:化學系所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2016
畢業學年度:104
語文別:英文
論文頁數:72
中文關鍵詞:溫莎拉
外文關鍵詞:Rudolf1711
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Linear alkyl benzene sulfonates (LAS) are the most commonly used anionic surfactants in household laundry. These compounds have alkyl chains from C10-C14. LAS toxicity towards agriculture soil further could be at a risk level, so that a sensitive and precise analytical method for the determination of their residual levels in agriculture soil is required by developing a method for their determination on vegetable. QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used for the extraction of linear alkyl benzene sulfonates from the vegetable. In order to establish an efficient method for the extraction of linear alkyl sulfonates in mixture standard solution, QuEChERS method was optimized, using various sorbent and solvent system combinations, followed by LC-MS/MS for the identification and quantification of LAS in vegetable samples. The best results were obtained using acetonitrile as the extraction solvent and 25 mg primary secondary amine (PSA) and 25 mg graphitized carbon black (GCB) as sorbent. The selection of specific fragmentation reaction for LAS allowed simultaneous quantification and identification by monitoring the ion at m/z 183 and 119.The limits of quantification were obtained
302.37 ng/mL (C10), 214.60 ng/mL (C11), 204.28 ng/mL (C12), 200.93 ng/mL (C13), 287.76 ng/mL (C14) and LOD were C10 1007.91 (C10) ng/mL, 908.22 ng/mL (C11), 744.10 ng/mL (C12) , 703.31 ng/mL (C13) , 811.7 ng/mL (C14).The correlation coefficients for the calibration curves was greater than 0.999 for all linear alkyl benzene sulfonates compound (C10-C14). A thorough optimization and validation of different amount of sorbent clean-up efficiency approaches was performed for the first time for the analysis of LAS. A spiked plant of LAS indicate that soil can absorb LAS (C10 – C14).




ACKNOWLEDGEMENT i
ABSTRACT ii
LIST OF CONTENT iii
LIST OF TABLES iv
LIST OF FIGURES v
INTRODUCTION 1
1.1 Linear Alkyl Benzene Sulfonates (LAS) 1
1.1.1 The Effects of LAS to Environment 4
1.1.2 Biodegradation Pathways 5
1.1.3 Analysis of Linear Alkyl Benzene Sulfonates (LAS) 6
1.2 QuEChERS 9
1.3 Water Spinach 10
1.4 Mass Spectrometry 11
1.4.1 Ionization Sources 12
1.4.2 Electrospray Ionization 12
1.4.3 Mass Analyzer 16
1.4.4 Quadrupole 16
1.4.5 Tandem Mass Analyzer 17
EXPERIMENTAL 22
2.1 Chemicals and Reagents 22
2.2 Preparation of Analytical Standards. 22
2.2.1 Stock Solution 22
2.2.2 Spike Solution 22
2.3 Instrumentation 23
2.3.1 Liquid chromatography 23
2.3.2 Mass spectrometry 23
2.4. Sample Preparation 23
2.4.1 Vegetable 24
2.4.2 QuEChERS 24
2.5. Method Validation 24
RESULTS AND DISCUSSION 26
3.1. Method development 26
3.1.1. Optimization of LC parameters 26
3.1.2. The chromatographic condition 28
3.1.3. Optimization of MS/MS condition 36
3.1.4. QuEChERS Optimization condition 50
3.2. Method Validation 56
3.3. Real Sample 64
CONCLUSION 67
REFERENCES 68





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