開發利用MALDI TOF/MS進行針對塑化劑的快速篩檢與半定量之偵測技術

The Development of High Throughput Screening and Semi-Quantitative Technique for Phthalate Esters by MALDI-TOF MS

林昶達(Chang-da Lin)

指導教授 ： 陳政男

朝陽科技大學/理工學院/應用化學系/碩士(2013年)

摘要

鄰苯二甲酸酯類（Phthalate Esters, PAEs）為塑膠常使用的塑化劑，因作用與合法食品添加劑中起雲劑內的棕櫚油類似，且成本低廉，因此有不肖業者將合法的食品添加劑中的棕櫚油替換成DEHP，使得食品中的塑化劑含量超過標準甚高，造成人心恐慌。目前官方公告食品類的檢測方法是使用LC-MS，相當的耗費時間與溶劑，對於未受汙染的樣品也須花費相同的成本，因此開發一個可大量且快速篩檢的技術搭配官方檢測方法，將未受塑化劑污染的樣品先篩選出來，只對受汙染的樣品進行定量分析，便可節省時間與成本的消耗，也符合綠色化學的環保概念。
本論文利用MALDI-TOF MS具有高通量、快速與高靈敏的特性開發了一個快篩的分析方法，以離子液體基質Et3N-α-CHCA取代傳統有機基質，以降低在低質量區時傳統有機基質的背景干擾，有利於檢測食品中塑化劑的殘留。此快篩方法主要針對市售果汁、運動飲料、果醬與茶類飲品，前處理只需將樣品經由甲醇萃取後離心，取上清液就可偵測，製備方法既簡單且成本低廉。利用MALDI-TOF MS的特性，本實驗可有效的偵測大量的樣品，針對當初事件中主要的6種塑化劑，果汁類只要濃度達0.5 ppm以上就都可檢測出來，之後再將受汙染的樣品篩檢出來後以官方的方法進行定量分析。一個樣品的偵測時間也小於1分鐘，對DEHP標準品也可測到1 ppb。論文中也對半定量方法進行探討，半定量主要分2種方法，一種為固定DIDP濃度所得的訊號強度當內標來與其餘塑化劑的訊號強度做比較，另一種為取一固定背景訊號當內標訊號來與6種塑化劑的訊號強度做比較，半定量的結果除了DINP與DBP因訊號強度問題不好定量外，其餘4種塑化劑根據2種不同的定量方式線性範圍分別為0.5 ppm～3 ppm(r 2 > 0.96)，0.5 ppm～2.5 ppm(r2 > 0.85)。

關鍵字

半定量 ； 基質輔助雷射脫附游離飛行時間質譜法 ； 塑化劑

並列摘要

Phthalate esters are often used as plasticizers; the function is similar to the role of palm oil in cloudy agent which is a food additive. DEHP is the most used plasticizer which is also a carcinogen. Others include DIDP, DINP, DBP, DEHP, BBP, DNOP. Because of its much low cost, plasticizers were used to replace palm oil and its excessive adding amount had caused the whole society involving in a huge food-safety crisis during the latter half of 2011. The official analysis method for plasticizers is using LC-MS/MS. It was quite time and solvent consuming, also is not convenient for a lot of samples analysis. Especially, the same cost will be wasted on uncontaminated samples. Therefore, to develop a low cost and high throughput screening method to filter out the uncontaminated or not excessive- contaminated samples may save cost and avoid second contamination to environment which is the trend of green chemistry.
In this study, we develop a low cost and high throughput rapid screening method by MALDI-TOF MS. Ionic matrix, Et3N-

並列關鍵字

semi-quantitative ； MALDI-TOF MS ； Plasticizer

參考文獻

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