臺灣博碩士論文加值系統

本次實驗採用“液相萃取”搭配 HPLC 來分析橄欖油塑化劑含量，目的是建立一個快速簡單的高效能液相層析儀-光電二極體陣列檢測器 (High-Performance Liquid Chromatography-Photo Diode Array Detector, HPLC-PDAD) 方法，不需要複雜的樣品前處理步驟，即可分析鄰苯二甲酸酯類 (phthalate esters, PAEs) 的化合物，進而分析較難處理的油樣品探討不同包材其釋放塑化劑含量，了解食用油的塑膠包裝材質是否會釋放或殘留塑化劑危害人類健康安全。首先進行塑化劑標準品定性分析，讓標準品完全分離後對其作檢量線，標準品包含鄰苯二甲酸二甲酯 (dimethyl phthalate, DMP)、鄰苯二甲酸二乙酯 (diethyl phthalate, DEP)、鄰苯二甲酸二丁酯 (di-n-butyl phthalate, DBP)、鄰苯二甲酸苯基丁酯 (benzylbutyl phthalate, BBP)、鄰苯二甲酸二 (2-乙基己基) 酯 (di-(2-ethylhexyl) phthalate, DEHP)、鄰苯二甲酸二辛酯 (di-n-octyl phthalate, DNOP) 具有0.033-16.66 (µg/ml)，R2 > 0.995 之良好線性範圍，偵測極限 (Limit of Detection, LOD) 為 0.01-0.13 (µg/ml) 及定量極限為 (Limit of Quantitation, LOQ) 0.03-0.26 (µg/ml)，進而作精密度試驗 (Relative standard deviation, RSD%)，如 : DEHP 最低可至 5% 範圍內。經 50 ± 2℃ 儲藏之 60 天橄欖油樣品，分別在自然及密閉組的 PET、HDPE 和 LDPE 等材質中，檢測到容器遷移釋放出 DMP 及 DEP 的含量，並介於 4.77-16.84 (µg/ml) 和 0.97-9.18 (µg/ml) 之間，其他四種鄰苯二甲酸酯類項目則未偵測到，綜合上述結果，本研究建立良好之六種塑化劑標準品分析步驟與結果，可增加樣品在此方面的準確度 (Accuracy)，並可快速簡單的檢測出油樣品經高溫儲藏後所遷移釋放之含量。

In this experiment, “liquid extraction”and HPLC are utilized to analyze the plasticizer content in olive oil. The goal of this experiment is to establish a fast and simple method of HPLC-PDAD (High-Performance Liquid Chromatography-Photo Diode Array Detector) that can analyze PAEs (phthalate esters) without complicated pretreatment.Then oil samples are analyzed to examine the effect of plasticizer content releasing in different packaging materials to understand the releasing or residual plasticizer of edible oil packaging, which is harmful to human health. First, the qualitative analysis of plasticizer standards is completed. After complete separation of standards, calibration curve is made. The standards includes DMP (dimethyl phthalate), DEP (diethyl phthalate), DBP (di-n-butyl phthalate), BBP (benzylbutyl phthalate), DEHP (di-(2-ethylhexyl) phthalate) and DNOP (di-n-octyl phthalate). All above PAEs are with well linear ranges which are 0.033-16.66 (µg/ml), R2 > 0.995, and the LOD (Limit of Detection) and LOQ (Limit of Quantitation) are 0.01-0.13 (µg/ml) and 0.03-0.26 (µg/ml), respectively. The precision test is finished (Relative standard deviation, RSD%) such that the least range of DEHP can reach to 5%. Through the 50 ± 2℃ storage test, the DMP and DEP migrated out of the containers including PET, HDPE and LDPE which sealed and without sealed were detected as the content are within 4.77-16.84 (µg/ml) and 0.97-9.18 (µg/ml) in the olive oil samples for 60 days. Other PAEs are not detected. Hence, this study established good standard operation protocols and analysis results of six standard plasticizers, leading to the accuracy for samples. Furthermore, the PAEs migrated out of the oil samples which were stored in high temperature can fast and simple be detected. A rapid and simple HPLC method is established to examine the release of the PAEs including DMP and DEP in the packaged olive oil from PET, HDPE and LDPE packaging materials during 60 days storage at 50 ± 2℃.

摘要 I
Abstract II
圖目次 V
表目次 VIII
壹、緒論 1
貳、文獻回顧 2
一、包裝食用油之簡介 2
二、塑化劑-鄰苯二甲酸酯類 2
(一) 鄰苯二甲酸酯類之物化特性及用途 3
1. 物化特性 3
2. 用途 3
(二) 國內外鄰苯二甲酸酯類之使用情形 3
1. 國外 3
2. 國內 4
(三) 鄰苯二甲酸酯類之國內外相關法規 4
1. 國內法規 5
2. 國外法規 5
(四) 鄰苯二甲酸酯類之毒性 6
(五) 食品含食用油中之鄰苯二甲酸酯類及其轉移之情形 7
(六) 鄰苯二甲酸酯類之相關分析方法 7
三、食品塑膠材質 9
(一) 聚苯乙烯 (Polystyrene, PS) 9
(二) 聚丙烯 (Polypropylene, PP) 9
(三) 聚乙烯 (Polyethylene, PE) 10
(四) 聚酯 (Polyester, PET) 10
(五) 聚偏二氯乙烯 (Polyvinyldichloride, PVDC) 10
参、實驗架構 12
肆、實驗材料方法 13
一、實驗材料 13
(一) 樣品 13
(一) 標準品及溶劑 13
(二) 儀器與設備 13
二、實驗方法 14
(一) 鄰苯二甲酸酯類標準品溶液製備 14
(二) 檢量線標準溶液製備 14
(三) 偵測極限及定量極限測定 14
(四) 分析方法精密度 14
(五) 儲藏試驗 15
(六) 樣品萃取 15
(七) 高效液相層析儀分析之條件 15
伍、結果 16
一、高效能液相層析儀分析條件最佳化條件 16
(一) 吸收波長選擇 16
(二) 移動相之選擇 16
二、 鄰苯二甲酸酯類濃度分析之定性分析、檢量線、定量極限、偵測極限和精密度 16
三、 放置不同包材之橄欖油於高溫下之儲藏試驗 17
四、 不同包材之橄欖油於高溫下儲藏兩個月之鄰苯二甲酸酯類遷移含量 17
(一) 一個月高溫儲藏下之容器遷移鄰苯二甲酸酯類至橄欖油內含量 17
(二) 二個月高溫儲藏下之容器遷移鄰苯二甲酸酯類至橄欖油內含量 18
陸、討論 20
一、 高效能液相層析儀分析條件最佳化條件探討 20
二、 鄰苯二甲酸酯類濃度分析之定性分析、檢量線、定量極限、偵測極限和精密度 20
三、 放置不同包材之橄欖油於高溫下之儲藏試驗 21
四、 探討不同包材之橄欖油於高溫下儲藏兩個月之鄰苯二甲酸酯類遷移量 21
柒、 結論 24
捌、 參考文獻 25
玖、 附錄 76

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