Llovera Montserrat, Balcells Mercè, Torres Mercè, Canela Ramon
Chemistry Department, Universitat de Lleida, Spain.
J Agric Food Chem. 2005 Aug 24;53(17):6643-8. doi: 10.1021/jf0513157.
The polymer-assisted reaction of 4-(hydroxymethyl)furan-2(5H)-one (4HM2F) with 21 carboxylic acids using polystyrene-carbodiimide (PS-carbodiimide) yielded an ester library. Four of the esters, (5-oxo-2,5-dihydrofuran-3-yl)methyl acetate (IS-1), (5-oxo-2,5-dihydrofuran-3-yl)methyl butyrate (IS-2), (5-oxo-2,5-dihydrofuran-3-yl)methyl 2-methylpropanoate (IS-3), and (5-oxo-2,5-dihydrofuran-3-yl)methyl chloroacetate (IS-4), were tested as internal standards for the quantification of patulin in apple juice by gas chromatography-mass spectrometry in the selected ion monitoring mode (GC-MS-SIM). The developed method combines an AOAC official extractive step and a GC-MS-SIM analysis. Using a chromatographic column containing trifluoropropylmethylpolysiloxane as the stationary phase and IS-1 as the internal standard, it was possible to perform an accurate and precise quantification of underivatizated patulin in apple juice at concentrations down to 6 microg/L. A detection limit of 1 microg/L was established.
使用聚苯乙烯 - 碳二亚胺(PS - 碳二亚胺),4 - (羟甲基)呋喃 - 2(5H) - 酮(4HM2F)与21种羧酸进行聚合物辅助反应,得到了一个酯类库。其中四种酯,乙酸(5 - 氧代 - 2,5 - 二氢呋喃 - 3 - 基)甲酯(IS - 1)、丁酸(5 - 氧代 - 2,5 - 二氢呋喃 - 3 - 基)甲酯(IS - 2)、2 - 甲基丙酸(5 - 氧代 - 2,5 - 二氢呋喃 - 3 - 基)甲酯(IS - 3)和氯乙酸(5 - 氧代 - 2,5 - 二氢呋喃 - 3 - 基)甲酯(IS - 4),在选择离子监测模式(GC - MS - SIM)下,作为气相色谱 - 质谱法测定苹果汁中展青霉素含量的内标进行了测试。所开发的方法结合了美国官方分析化学师协会(AOAC)的官方提取步骤和GC - MS - SIM分析。使用以三氟丙基甲基聚硅氧烷为固定相的色谱柱,并以IS - 1作为内标,可以对苹果汁中浓度低至6微克/升的未衍生化展青霉素进行准确而精确的定量。确定了1微克/升的检测限。