油脂中五種合成抗氧化劑之系統分析   全文下載

Simultaneous Determination of Five Synthetic Antioxidants in Fats and Oils

利用逆相高效液相層析法（RP-HPLC），分析食用油脂中沒食子酸丙酯（PG）、第三丁基氯?（TBHQ）、NDGA、丁基羥基甲氧苯（BHA）及二丁基羥基甲苯（BHT）五種抗氧化劑之系統檢驗方法業已經本研究建立。其主要分析步驟為檢品溶於正戊烷，取一定量注入固相抽出分離管（Adsorbex RP-18）並收集流出液。該固相抽出分離管再用溶離液 （2-Propanol／Acetonitrile = 1：1）每次1 ml分別沖洗三次收集溶出液；合併流出液及溶出液並以溶離液加至4 ml供作檢液。注入定量之檢液於逆相高效液相層析儀中（管柱μ-Bondapak C18）同時做五種合成抗氧化劑之定量分析。取一定量之沒食子痠丙酯、第三丁基氫?、NDGA、丁基羥基甲氧苯及二丁基羥基甲苯標準品混合溶解後，分別添加於各種食用油脂中，經測試結果其回收率分別為92.0～98.1%，92.2～99.9%，98.8～100.7%，90.5～97.1%及91.0～97.0%。上述五種抗氧化劑其濃度範園在2.5-20μg／ml範圍內，任取五種濃度加以測試，其標準曲線及檢量線均能維持良好之線性關係。本系統檢驗法不僅操作簡便，溶媒的使用量大減，並具良好的線性關係及回收率，在對食用油脂進行上述五種抗氧化之同時分析時效果亦十分卓越。

A high-performance liquid chromatographic (HPLC) method for simultaneous determination of gallic acid n-propyl ester (PG), tert-butyl hydroquinone (TBHQ), nor-dihydroquaiaretic acid (NDGA), 3-tert-butyl-4-hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in fats and oils was developed. The samples were dissolved in n-pentane. Aliquot (1 ml) of the pentane solutions was pipetted onto Adsordex RP-18 extraction column (400 mg). The antioxidants were eluted with three 1-ml portions of acetonitrile/2- propanol (1:1). The filtrate and the eluate were collected and mixed. The final volume was adjusted to 4 ml with acetonitrile/2-propanol and determined by HPLC with a UV detector set at 280 nm. The recoveries of PG, TBHQ, NDGA, BHA and BHT fortified to various edible fats and oils were in the range of 92.0～98.1%, 92.2～99.9%, 98.8～100.7%, 90.5～97.1% and 91.0～97.0%, respectively. Each of the standard and calibration curves for PG, TBHQ, NDGA, BHA and BHT showed a good linear relationship in the range of 2.5～20 ppm.