利用聚十八烯二乙烯苯整體成形管柱之毛細管電層析方法分析磺胺類藥物

Sulfonamide Analyses by Capillary Electrochromatography using Poly(octadecene-divinylbenzene) Monolithic Column

林正藍(Cheng-Lan Lin)

指導教授 ： 黃悉雅

中原大學/理學院/化學研究所/碩士(2009年)

https://doi.org/10.6840/cycu200901181

摘要

本論文進行毛細管電層析(capillary electrochromatography, CEC)技術的研究，分為兩部分討論，第一部分討論有機高分子整體成形管柱(monolithic column)之開發。製備新型態高分子聚十八烯二乙烯苯(POD-DVB)靜相，並且以帶正電荷單體vinylbenzyl trimethylammounium(VBTA)做為提供電滲流之來源。將所製備出之整體成形管柱應用在毛細管電層析技術上，分離八種磺胺類藥物。藉由改變靜相中帶電荷單體比例、單體含量變化、減少管柱有效長度以及動相乙腈含量，可在15分鐘內完成八種磺胺類藥物之分析。最後測試此CEC方法結合階段式梯度沖提(step gradient elution)與線上樣品濃縮(on-line sample concentration)技術，探討磺胺類分析之效能。研究顯示階段式梯度沖提方法可改善分析物拖尾的情形，並且將分析時間由原本15分鐘縮短至11分鐘內。而結合線上樣品濃縮技術，可降低磺胺類化合物的偵測極限約200倍左右，偵測極限範圍在9.2-28.2 ng/mL。當此方法應用在食品檢測上，可成功檢測牛奶樣品中的磺胺類化合物。
論文第二部分討論填充式管柱之製作，選擇PS-DVB共聚物做為擋板(最佳擋板長度為2 mm)，及用C18做為填充之靜相。結果顯示可成功製備良好再現性CEC管柱，滯留時間之再現性範圍在1.25-3.04 % (n=3)。將此C18填充式管柱應用在鄰苯二甲酸酯類的分析上，再結合階段式梯度沖提法後，可使分析時間由70分鐘縮短至18分鐘。

關鍵字

整體成形管柱 ； 毛細管電層析

並列摘要

In the thesis, capillary electrochromatography (CEC) technique was studied and divided into two parts. In the first-part of the study, development of organic polymer-based monolithic column was investigated. Poly(octadecene- divinylbenzene) (POD-DVB) was preparaed as novel stationary phase, which using vinylbenzyl trimethyammonium (VBTA) as charge-carried monomer provided EOF. The monolithic column was applied to eight sulfonamides separation by CEC. The effect of the polymerization condition of the stationary phase (ratios of charged-carried monomer, monomer level, effective length) and acetonitrile content in the mobile phase were examined. The separation of eight sulfonamides was completed in 15 min.. Finally, the CEC method coupled step gradient elution or on-line sample concentration which were examined for the separation efficiency of sulfonamides.
The research indicated that step gradient elution was effective in reducing the peak tailing, and the separation time was shortened from 15 to 11 min.. The combination of on-line sample concentration detection limit of sulfonamide compounds was improved to about 200 times. The detection limit was in the range of 9.2 to 28.2 ng/mL. This method has been applied to food analyses. A trace amount of sulfonamide in milk was detected successfully.
In the second-part of thesis, preparation of packed column was studied. Frits were prepared by using PS-DVB co-polymer (the optimum length was about 2 mm), and C18 silica was taken in as the stationary phase in packed column. The result showed that CEC packed column with good reproducibility was successfully prepared. The reproducibility of retention time was in the range 1.25 to 3.04 % (n=3). The C18 packed column was applied to the analyses of phthalate acid esters (PAEs), which combined with step gradient elution. The separation time can be shortened from original 70 to 18 min. when compared to isocratic elution.

並列關鍵字

monolithic column ； capillary electrochromatography

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