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目的建立固相萃取-三重串联四极杆气相色谱/质谱联用(GC-MS/MS)同时测定16种邻苯二甲酸酯类化合物的分析方法。方法样品加乙腈涡旋、超声提取、离心分离后经固相萃取仪净化,采用三重串联四极杆气相色谱/质谱联用在多反应监测模式(MRM)下进行测定。结果在MRM模式下用两对离子对16种邻苯二甲酸酯类进行分析,基线漂移少,且在5 V~40 V能量范围内,对母离子进行了碰撞能量优化;16种邻苯二甲酸酯类线性范围为6.0μg/L~5000μg/L,线性相关系数在0.9900~0.9994之间,检出限为0.01 mg/kg~0.04 mg/kg,定量限为0.03 mg/kg~0.1 mg/kg,平均加标回收率为70.1%~119.8%,相对标准偏差(RSD)均<10%。结论该方法适合食用油中邻苯二甲酸酯类的测定,具有良好的回收率及稳定性。
Objective To establish a method for the simultaneous determination of 16 phthalate esters by solid-phase extraction coupled with triple quadrupole gas chromatography-mass spectrometry (GC-MS / MS). Methods The sample was vortexed with acetonitrile and extracted by ultrasonic. After centrifugation, the samples were purified by solid phase extraction (SPE) and determined by multi-reaction monitoring (MRM) with triple quadrupole GC / MS. Results In the MRM mode, 16 kinds of phthalates were analyzed by two pairs of ions with less baseline drift, and the collision energies of precursor ions were optimized in the energy range of 5 V ~ 40 V. 16 kinds of phthalic acid esters The linear range of the formate ranged from 6.0μg / L to 5000μg / L, the linear correlation coefficient ranged from 0.9900 to 0.9994, the limit of detection ranged from 0.01 mg / kg to 0.04 mg / kg, and the limit of quantification ranged from 0.03 mg / kg to 0.1 mg / kg, the average recovery was 70.1% ~ 119.8%, the relative standard deviation (RSD) were <10%. Conclusion This method is suitable for the determination of phthalates in edible oils and has good recovery and stability.