臺灣博碩士論文加值系統

Nitrobenzene類化合物是種高毒性物質，對環境會造成污染。由於此類衍生物具染色特性，因此常被應用於染料工業上。本研究為探討利用膠束電動層析法(MECC)及高效能液相層析法(HPLC)的分析技術來測定十二種含氫氧基及胺基nitrobenzene類化合物，將建立高精密度和高準確度的定性及定量方法。
MECC最佳分離條件是緩衝溶液組成為在23mM四硼酸鈉溶液內添加50mM sodium dodecyl sulphate (SDS) 及10% ethanol (EtOH)，融矽毛細管為75mm I.D.´75cm(50cm) ，電場強度為230V/cm。遷移時間與積分面積再現性分別低於1.65%及4.22%，線性範圍為0.3~60mg/mL，線性相關係數0.9904以上，偵測極限為0.1~0.7mg/mL。而MECC最大特點是可以分離會破壞HPLC管柱之對氫氧基硝基苯化合物。且藉由加入50mM cetyltrimethylammonium chloride(CTAC)下，可將胺基nitrobenzene類化合物完全分離。
HPLC最佳分離條件為C18的層析管柱，以含6% Tetrahydrofuran (THF) 及10mM ammonium dihydrogen phosphate (pH6.0)水溶液及methanol 梯度沖提。
結果為HPLC分析時間較短(12min)、再現性(RSD<2.87)較好，MECC有較廣之線性範圍。
最後將HPLC及MECC的分離技術，以直接分析法及標準添加法實際應用到市售染髮劑。所得結果之回收率均高於90%、再現性則小於3.6%。

Nitrobenzenes, carcinogen pollutants, are widely used in dye industries. An analytical method of twelve nitrobenzene compounds with hydroxyl group and/or amino group will be established by micellar electrokinetic capillary chromatography (MECC) and high performance liquid chromatography (HPLC) in this study.
The optimum condition for MECC is 50mM sodium dodecyl sulphate and 10% ethanol in 23mM sodium borate buffer solution, 75mm (I.D.)´75cm (efficient length 50.0cm) fused-silica capillary and 230V/cm electric field strength. Under this condition, good linear range (0.3~60mg/mL ), acceptable correlation coefficient (>0.9904), and detection limit (0.1~0.7mg/mL) were obtained. The advantage is para-hydroxyl nitrobenzenes can be separated by this condition. By the way nitroaniline isomers can be separated completely by addition of cationic surfactant, cetyltrimethylammonium chloride.
The optimum analytical condition of HPLC is 6% tetrahydrofuran in 10mM ammonium dihydrogen phosphate (pH6.0) aqueous and methanol as mobile phase with C18 analytical column. The shorter analytical time (12min) is obtained by gradient elution. The good resolution(Rs=1.34) and acceptable reproducibility(RSD<2.87) were obtained.
The proposed analytical techniques of HPLC and MECC were applied to several commercial hair dyes products with direct analysis and standard addition method. The results of recovery(>90%), and reproducibility (RSD<3.6)were obtained.

目錄 ........................................I
謝誌 ........................................III
中文摘要 ....................................IV
英文摘要 .....................................V
圖目錄 .......................................VI
表目錄 .......................................IX
第一章 緒論 ..................................1
第一節 研究目的 ...............………………....1
第二節 染髮劑之分類 ......................… .1
第三節 染髮劑毒性 ......................……….2
第四節 化合物性質 ........................…….5
第五節 文獻記載之分析方法 .....................8
第二章 高效能液相層析法 ........................18
第一節 原理 .............................18
一. 依作用機制分類………………………………19
二. 儀器架構 ......................20
第二節 實驗部份 ...........................22
一. 儀器設備 ......................22
二. 藥品 ..........................23
三. 藥品配製 ......................24
四. 定性依據 ......................24
第三節 結果與討論 ........................26
一. 定性分離條件之建立…………………………..28
二. 定量 ....................................35
第三章 毛細管電泳法 ............................….38
第一節 毛細管電泳原理 ......................…38
一. 發展簡介 .....................….38
二. 毛細管電泳之分離原理..............…39
三. 影響分離效率的因素 ................43
四. 操作模式 .........................44
第二節 實驗部份 ..........................….49
一. 儀器設備 ......................….49
二. 藥品 ..........................….49
三. 藥品配製 .......................….49
四. 毛細管之清洗方式 ..................50
第三節 結果與討論 ..........................….50
一. 建立最佳定性分析條件 ..............……51
二. 定量 ...............................….62
第四章 高效能液相層析法與毛細管電泳法之比較 ..........…66
第五章 市售染髮劑之檢測 …………………………………………69
第六章 結論 ………………………………………………………..75
第七章 參考文獻 …………………………………………………..77

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