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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。
The ultrasonic extraction of 17 kinds of phthalates in concentrated fruit juice was established by solid phase extraction and gas chromatography / mass spectrometry. The sample was extracted with n-hexane by sonication and purified by solid phase extraction with ethylenediamine-N-propylsilane (PSA). The sample was separated on a VF-5MS column (30 m × 0.25 mm × 0.25 μm) and analyzed by gas chromatography / mass spectrometry Analysis by selective ion storage (GC / MS / SIS). The results showed that 17 kinds of phthalates showed a good linearity in the range of 0.05 mg / L ~ 10.00 mg / L, the correlation coefficients were all greater than 0.998, the recoveries of three kinds of phthalates were between 80% and 110% The RSDs ranged from 0.5% to 7.6%. The detection limits of 17 target compounds ranged from 0.01 mg / L to 0.50 mg / L. The method is rapid and accurate, with less background interference and high analytical sensitivity. It is suitable for the analysis of phthalates in concentrated fruit juices.