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目的建立GC-MS/MS法测定食用植物油中17种邻苯二甲酸酯类化合物(PAEs)的方法。方法样品经正己烷溶解,WelchromO-PTC玻璃混合型固相萃取柱净化,乙酸乙酯洗脱,洗脱液用氮气吹干,正己烷定容,气相色谱-三重串联四级杆质谱(GC-MS/MS)联用法测定,外标法定量。结果 17种PAEs的加标回收率为65.9%~103.8%之间,相对标准偏差在1.08%~7.23%(n=6)之间,方法的检测限在0.001 mg/kg~0.02 mg/kg之间。市售的20份塑料桶装食用植物油中检出邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基)己酯(DEHP),检出率分别为20%(4/20)、5%(1/20)、10%(2/20)、25%(5/20)、25%(5/20),含量范围分别为<0.004 mg/kg~0.2 mg/kg、<0.004 mg/kg~0.1 mg/kg、<0.003 mg/kg~4.0 mg/kg、<0.003 mg/kg~1.6 mg/kg、<0.005 mg/kg~7.8 mg/kg。结论本方法简便、快速、灵敏度高,适用于食用油中邻苯二甲酸酯定性和定量测定。
Objective To establish a method for the determination of 17 phthalate esters (PAEs) in edible vegetable oils by GC-MS / MS. Methods The sample was dissolved in n-hexane, purified on a WelchromO-PTC glass-mixed solid-phase extraction cartridge and eluted with ethyl acetate. The eluent was blown dry with nitrogen, fixed with n-hexane and analyzed by gas chromatography-triple quadrupole mass spectrometry GC-MS / MS) combined with external standard method of quantification. Results The spiked recoveries of 17 PAEs ranged from 65.9% to 103.8% with relative standard deviations between 1.08% and 7.23% (n = 6). The limits of detection were within the range of 0.001 mg / kg to 0.02 mg / kg between. Commercially available 20 plastic bottled edible vegetable oil detected in the detection of dimethyl phthalate (DMP), diethyl phthalate (DEP), di-isobutyl phthalate (DIBP), o- DBP and DEHP were detected in 20% (4/20), 5% (1/20), 10% (2) / 20), 25% (5/20) and 25% (5/20), respectively, in the range of 0.004 mg / kg to 0.2 mg / kg and 0.004 mg / kg to 0.1 mg / kg to 4.0 mg / kg, <0.003 mg / kg to 1.6 mg / kg, <0.005 mg / kg to 7.8 mg / kg. Conclusion The method is simple, rapid, sensitive and suitable for the qualitative and quantitative determination of phthalates in edible oil.