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研究生:林秀慶
研究生(外文):Lin, Show-Ching
論文名稱:無孔性矽膠為吸附劑之親水性層析
論文名稱(外文):Non-Porous Aminopropyl-Silica for Hydrophilic Interaction Chromatography
指導教授:李文乾
指導教授(外文):Wen-Chien Lee
學位類別:碩士
校院名稱:國立中正大學
系所名稱:化學工程研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:1997
畢業學年度:85
語文別:中文
論文頁數:61
中文關鍵詞:無孔性矽膠親水性層析
外文關鍵詞:non-porous silicahydrophilic interaction chromatography
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對於醣類的親水性層析最廣泛被使用的是化學鍵結丙基胺的固定相所
充填的管柱以及配合氰甲烷-水的混合組成為動相溶液,而市售的管柱所
充填的均為多孔性吸附劑,因有溶質進出孔洞的質傳效應所以需要較長的
沖提時間。當無孔性吸附劑使用管柱的充填材料時,在相同流速之下樣品
很快的被沖提出來。 本
研究為自行製備無孔性矽膠為吸附劑,無孔性矽膠的粒徑約為3.04 μm,
利用α-胺基丙基三乙氧甲矽烷將無孔性矽膠表面矽烷化使丙基胺鍵結於
其上,胺基的鍵結量為1.98 μmole/m2,可確定為單層矽烷化。再由所製
備的丙基胺-矽膠西附劑充填成5cm×0.46cm I.D.及10cm×0.46cmI.D.兩
支管柱,分別測試其分離醣類的層析行為. 由實驗結果顯示在5公分管柱
分離葡萄糖及乳糖時若以流量0.5 ml/min操作,只須3分多鐘即可分離完
全 ,從滯留時間對5μl試樣中葡萄糖濃度的變化關係可得知此管柱之
最大樣品負載為5μg,當葡萄糖濃度為0.1mg/l時尚能檢測出其存在,因此
此管柱較適於低容量樣品環或低濃度試樣分析。流量在0.35ml/min有其較
低的理論板高,當流量高於0.35ml/min則流量增加板高隨之增加。以10cm
×0.46cm I.D.管柱與市售多孔性吸附劑之管柱分離β-fructofuranosi
dase催化蔗糖生成果寡糖的產物,10公分管柱以流量0.5ml/min需時約8分
鐘可完成分離, 市售管柱約24分鐘,在分離的時間上確實較快。10公
分管柱在流量0.3ml/min時有其最小 的理論板高,當流量超過0.3ml/
min,板高隨流量增加而增加。本研究所製備之管柱對果糖與蔗糖的分離
效果仍不理想,這是因為管柱的吸附 容量較小所致.



Chemically bonded aminopropyl silicas are the most widely
used for the hydrophilic interaction chromatography of
carbohydrates. The mobile phases consisting of acetonitrile-
water mixture are usually employed. All of the commercial
columns used for carbohydrate chromatography are packed with
porous sorbents. In a column packed with porous sorbent, mass
transfer effects due to pore diffusion of solutes into and out
of the sorbent may result in a longer elution time.
However, when non -porous silica sorbents are employed as
packing materials. The solutes can be rapidly separated on the
column.

In this research, the non-porous silica having an average
diameter of 3.04 μm was prepared . The non-porous silica
was silanlized with α-aminopropyltriethoxy silane to
introduce terminal amino groups with a densityof 1.98 μmole/m2
on the surface. It is believed that the modified silicacovered a
monolayer of silane on its surface. The resultant aminopropyl-
silicasthen were packed into two columns (5 cm×0.46 cm I.D. and
10 cm×0.46 cm I.D.). The mixture of glucose and lactose
could be separated in 3 min in the 5-cm long column at a flow
rate of 0.5 ml/min. The maximum loading capacity of this column
was determined to be 5 μg. A sample with a glucose
concentration down to 0.1 mg/l could be quantitatively
analyzed. The results indicated that the column was suitable
for analysis of low sugar concentrations. The lowest value of
plate height could be reached by reducing the flow-rate to
0.35 ml/min .The 10-cm long column was effective for the
separation of fructo-oligosaccharides produced from sucrose
solution catalyzed by β-fructofuranosidase. The separation on
the 10-cm long column was accomplished in 8 min at a flow-rate
of 0.5ml/min . Whereas it took 24 min to conclude the
separation of fructo -oligosaccharides products on the
Supelcosil LC-NH2 column (25 cm×0.46 cm I.D.) with a flow-rate
of 1ml/min. However, due to the low bindingcapacity of the
prepared column, fructose could not be effectively
separatedfrom sucrose.



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