气相色谱/质谱法测定浓缩果汁中的邻苯二甲酸酯

Gas Chromatography/Mass Spectrometry for the Determination of Phthalic Acid Esters in Concentrated Fruit Juice

建立了浓缩果汁中17种邻苯二甲酸酯的超声提取—固相萃取净化—气相色谱/质谱分析方法。样品用正己烷超声提取,经乙二胺-N-丙基硅烷(PSA)固相萃取剂净化,经VF-5MS色谱柱(30 m×0.25 mm×0.25μm)分离,运用气相色谱/质谱联用选择离子存储法(GC/MS/SIS)进行分析。结果表明:17种邻苯二甲酸酯在0.05 mg/L～10.00 mg/L范围内线性良好,相关系数均大于0.998,三个水平的样品添加回收率在80%～110%之间,精密度(RSDs)在0.5%～7.6%之间,17种目标化合物的检出限为0.01 mg/L～0.50 mg/L。该方法快速准确、背景干扰较少、分析灵敏度较高,适用于浓缩果汁中邻苯二甲酸酯的分析。

A method based on ultrasonic extraction,solid phase extraction purification and gas chromatography/mass spectrometry was developed for the determination of 17 phthalic acid esters in concentrated fruit juice.Samples were extracted by hexane in an ultrasonic bath and the extract was purified with primary secondary amine（PSA）.Analytes were separated by VF-5MS column（30 m×0.25 mm×0.25 μm） and then identified and quantified by GC/MS/SIS method.The results showed that linearity of response over 17 phthalic acid esters was good from 0.05 to 10.00 mg/L with correlation coefficients higher than 0.998.The relative standard deviations（RSDs） were in the range of 0.5%~7.6%.Recoveries ranged from 80% to 110% for all compounds at three different spiked levels.The limits of detection were（0.01~0.50） mg/L.The method described here is rapid,accurate and suitable for the determination of phthalic acid esters in concentrated fruit juice.