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研究生:黃思萍
研究生(外文):Shih-Ping Huang
論文名稱:以高效能液相層析法和毛細管電泳法測定Stilbenes分析技術之研究
論文名稱(外文):Study on the analytical techniques of Stilbenes by high performance liquid chromatography and capillary electrophoresis
指導教授:王書蘋
指導教授(外文):Shu-Ping Wang
學位類別:碩士
校院名稱:靜宜大學
系所名稱:應用化學系
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:1999
畢業學年度:87
語文別:中文
論文頁數:97
中文關鍵詞:螢光增白劑毛細管電泳高效能液相層析直接分析標準添加法Stilbene
外文關鍵詞:Stilbenesfluorescent whitening agentcapillary electrophoresishigh performance liquid chromatographyanalysis of household
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Stilbene類化合物廣泛應用於清潔工業,其具有螢光增白之功能。本研究將針對這類化合物,如︰4,4¢-diaminostilbene-2,2¢-disulfonic acid, 4,4¢-bis[(4-anilino-6-morpholino-1,3,5-trazin-2-yl)amino]stilbene-2,2¢-disulfonate, 4,4¢-bis(2-sulfostryl)-biphenyl, 4,4¢-bis[(4-sulfoanilino)-6-bis(2-hydroxyethyl)amino-1,3,5-trazin-2-yl)amino]-stilbene-2,2¢-disulfonate, 4,4¢-bis[(4-anilino-6-methoxy-1,3,5-trazin-2-yl)amino]stil-bene-2,2¢-disulfonate and 4,4¢-bis[(4-anilino-6-methylamino-1,3,5-trazin-2-yl)amino]stilbene-2,2¢-disulfonate六種化合物,利用毛細管電泳 (Capillary Electrophoresis, CE)及高效能液相層析(High Perfo-rmance Liquid Chromatography, HPLC),建立高精密度和高準確度的定性及定量分析方法。而CE為首次應用於Stilbene類化合物之分離。
HPLC以C18當作層析管柱,移動相組成為離子試劑﹙tetrabutyl-ammoniumhydrogen sulfonate, TBA)水溶液與氰甲烷,可得到良好的分離。線性範圍為7.0’10-3 ~ 3.0’10 mg/mL,線性相關係數0.999以上,偵測極限為6 ~ 13 ng/mL。
CE的最佳分離條件為融矽毛細管75公分,緩衝溶液組成為含10.0 mM n-tetradecyltrimethylammonium borimide (TTAB) 及40%氰甲烷的50.0 mM tris(hydroxymethyl)aminomethane (TRIS)。可得到線性範圍為5.0’10-1 ~ 4.0’10 mg/mL,線性相關係數0.997以上,偵測極限為337~ 446 ng/mL。
除比較兩種方法之優缺點外,並將所建立之方法實際應用至市售商品 ? 洗衣清潔劑之分析。且將比較毛細管電泳與高效能液相層析、直接分析與標準添加法之結果,經由統計計算,兩種方法之結果在95% confidence level下並無明顯的差異,故可證明本研究分析方法之可靠性。

Stilbenes, fluorescence whitening agents(FWAs), are usually added into cleaning agent in household and in industry. Capillary electrophoresis (CE) was often applied to separate various compounds simultaneously for its multinomial advantages. Therefore, a analytical method for six stilbenes, namely, 4,4¢-diaminostil-bene-2,2¢-disulfonic acid, 4,4¢-bis[(4-anilino-6-morpholino-1,3,5-trazin-2-yl)amino]stilbene-2,2¢-disulfonate, 4,4¢-bis(2-sulfostryl)-biphenyl, 4,4¢-bis[(4-sulfoanilino)-6-bis(2-hydroxyethyl)amino-1,3,5-trazin-2-yl)amino]-stilbene-2,2¢-disulfonate, 4,4¢-bis[(4-anilino-6-methoxy-1,3,5-trazin-2-yl)amino]stilbene-2,2¢-disulfonate and 4,4¢-bis[(4-anilino-6-methylamino-1,3,5-trazin-2-yl)amino]stilbene-2,2¢-disulfonate, will be established by CE and high performance liquid chromatography (HPLC) in this paper.
The optimum mobile phase for HPLC was 4 mg/mL tetrabutylammo-nium hydrogen sulfate aqueous solution and acetonitrile. The good linear range(7.0’10-3 ~ 3.0’10 mg/mL); correlation coefficient (0.9992~ 0.9999) and detection limit(6~13 ng/mL) were obtained for six FWAs. And the optimum condition for CE was 10.0 mM n-tetradecyltrimethylammonium bromide and 40% ACN in 50.0 mM TRIS buffer solution, the fused-silica 75 cm (efficient length 50 cm) as capillary and electric field strength -280 V/cm. The linear range (5.0’10-1 ~ 4.0’10 mg/mL), correlation coefficient (0.9975~0.9998) detection limit (337~446ng/mL). Above 95% confidence level were obtained by comparison the results between direct and standard addition analysis.
The optimum analytical methods of CE and HPLC were applied to commercial products with direct analysis and standard addition.

目錄 .................................. ................. ................................................ I
謝誌 .................. ...................................... ........................................... III
中文摘要 .......................... ................. ............................................... IV
英文摘要 .......................... ..................... ............................................ V
表目錄 ................................ .............................................. ................. VI
圖目錄 ................................. ................................. .............................. IX
第一章 緒論 ....................... .................................................. ........... 1
第一節 螢光增白劑的發展過程 ........................ ................... 1
第二節 螢光增白之簡介 .......................... .............................. 1
一. 增白原理 ... ........................... ...................................... 1
二. 異構化過程 ............................ ...................................... 3
三. C.I.71, C.I.28和BSBP的光解過程及產物 ................... 3
第三節 螢光增白劑的分類 .............. ......................................... 4
第四節 Stilbenes的性質 ............... .............................................. 5
第五節 文獻記載的分析方法 ........... ....................................... 6
一. TLC ........................... .................................................. 7
二. HPLC .................................. ........................................... 8
第六節 實驗動機 ...................... ................................................. 14
第二章 高效能液相層析法 .............. .............................................. 15
第一節 原理 ............................ .................................................. 15
一. 管柱特性 ................... ..................................................... 16
第二節 實驗部份 ........................... ............................................ 17
一. 儀器設備 .................. ..................................................... 17
二. 藥品 ............................. ................................................. 18
三. 藥品配製 ....................... ................................................. 19
四. 定性與定量之判斷依據 ................ ............................... 19
第三節 結果與討論 ........................... ........................................ 21
一. 利用梯度沖提尋找最佳分離條件 .... ............................. 22
二. 線性範圍 ....................... ...................................................... 30
三. 校正曲線 ............... ............................................................. 31
四. 偵測極限 .................. ......................................................... 32
第三章 毛細管電泳法 .............. ....................................................... 33
第一節 原理 ............. .................................................................. 33
一. 電泳 ..................... ......................................................... 33
二. 電滲流 .............................. .............................................. 36
三. 電滲流的特性 ............................ .................................... 38
四. 電泳流 ........................... .................................................. 40
五. 焦耳熱生成與溫度梯度 ...... ....................................... 41
六. 七種分離機制 ...................... ......................................... 43
七. 影響分離效率的因素 .................... ............................. 50
第二節 實驗部份 ...................... ................................................. 55
一. 儀器設備 ..................... .................................................. 55
二. 藥品 ................... ............................................................ 55
三. 藥品配製 ......................... .............................................. 55
四. 毛細管清洗步驟 ................... ........................................ 56
第三節 結果與討論 .............................. ..................................... 57
一. 定性: 尋找最佳分離條件 ...................... ...................... 58
二. 定量 ......................... ....................................... ................ 68
第四章 高效能液相層析法與毛細管電泳法之比較 .................. 70
第五章 市售商品之檢測 .............................. ................................... 72
一. 前處理步驟 ................... ....................................................... 72
二. 結果 ............................ .......................................................... 72
第六章 結論 ................................. ..................................................... 80
第七章 參考文獻 ................................ ............................................... 81

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