液相微萃取結合毛細管電泳進行防腐劑之分析與線上濃縮結合毛細管電泳對三聚氰胺衍生物的偵測

Liquid-phase microextraction combined with capillary electrophoresis for preservative analyses, and determination of melamine derivative by on-line concentration coupled to capillary electrophoresis

陳冠廷(Kuan-Ting Chen)

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/cycu200901406

摘要

本研究第一部份為液相微萃取(Liquid-phase microextraction, LPME)技術結合毛細管電泳進行防腐劑系列化合物的檢測。實驗中以聚丙烯為材質的膜為萃取液膜，實驗過程藉由攪拌速度不同、接受相與供給相的pH值變化、接受相與供給相的種類與濃度變化、萃取溶劑的種類不同以及萃取時間變化，探討萃取效果。由實驗得知，以辛醇作為萃取溶劑，供給相溶液中使分析物不帶電荷，接受相溶液中使分析物帶電荷，有最好的萃取效果，並應用在實際樣品紅酒與醬油，藉此實驗技術可同時達到純化、濃縮等步驟，降低偵測極限。
第二部份則討論線上樣品濃縮技術(on-line sample concentration)結合微胞電層析(micellar electrophoresis capillary chromatography, MEKC)進行三聚氰胺系列化合物檢測。實驗中以反向電極極性堆積模式(reversed electrode polarity stacking mode, REPSM)分析三聚氰胺衍生物，並探討樣品堆積時間、樣品注射時間、樣品基質以及界面活性劑濃度等因素，對分離與堆積效果的影響。再以CSEI-sweeping-MEKC掃略式鹼水段的濃縮技術分析三聚氰胺，探討鹼水段長度、離子濃度等因素，對分離與堆積效果的影響。上述兩種線上濃縮方法可成功將三聚氰胺系列化合物分離與降低偵測極限。

關鍵字

三聚氰胺 ； 反向電極極性堆積 ； 陽離子掃略微胞電層析

並列摘要

The first part of this research used a liquid-phase microextraction (LPME) technique coupled to capillary electrophoresis (CE) to determine three preservatives. Polypropylene membrane was used as extraction medium in the experiment. Several parameters including stir speed, pH and solution type of donor phase and acceptor phase, and extraction time were examined in order to achieve optimal extraction. Octanol was used as the organic solvent. A basic acceptor phase (100 mMNaOH) should be used to promote dissociation of the acidic analytes, while acidic donor phase (10 mMHCl) could achieve good extraction by neutralizing the analytes. The study demonstrated that this LPME provided efficient preservative extraction in several samples (wine and soy sauce).
In the second part, two on-line sample concentration methods were coupled individually with micellar electrokinetic chromatography (MEKC) for melamine detections. First, a reversed electrode polarity stacking mode (REPSM) was developed. Effect of several factors such as sample stacking time, sample injection length, sample matrix and surfactant concentration on separation and stacking ability were examined. All analytes except for melamine could be detected successfully with the REPSM-MEKC method. Next, a cation-selective exhaustive injection and sweeping (CSEI-sweeping) method was also developed. The composition and length of water plug, and ionic strength of basic plug were optimized. Trace-level melamine (LOD 2.79 ppb) could be detected successfully with CSEI-sweeping MEKC method. Finally, the two on-line concentrations were also applied to determine melamine residual in food container made by melamine resins.

並列關鍵字

CSEI-sweeping-MEKC ； melamine ； REPSM

參考文獻

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