GC-MS/MS法测定食用植物油中17种邻苯二甲酸酯类化合物

Determination of 17 phthalic acid esters in edible vegetable oil by GC-MS /MS

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,WelchromO-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 determination of 17 phthalate acid esters（PAEs） in edible vegetable oil by gas chromatography tandem mass spectrometry （ GC -MS/MS）. Methods The sample was dissolved by n - hexane, cleaned by Welchrom O -PTC solid phase extraction cartridge, then the analyte was eluted by ethyl acetate and the eluted solution was dried by nitrogen gas. The residue was reconstituted with n - hexane and analyzed by GC - MS/MS, while external standard method was used for quantitative analysis. Results The spiked recoveries of 17 PAEs were 65.9% - 103.8% with RSDs of 1.08 % - 7.23 % （ n = 6）. The method detection limits were 0.001 mg/kg - 0.02 mg/kg. In 25 plastic buckets of edible vegetable oil, DMP, DEP, DIBP, DBP and DEHP were detected over the range of 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 and the detection rates were 20% （4/20）, 5% （1/20）, 10% （2/20）, 25% （5/20）, 25% （5/20）. Conclusion The method is convenient, speedy and high sensitive, and it is suitable for qualitative and quantitative analysis of phthalate acid esters in edible vegetable oil.