气相色谱-串联质谱法测定大豆提取物中16种多环芳烃和16种邻苯二甲酸酯类

Determination of 16 kinds of PAHs and 16 kinds of PAEs in soybean extract by gas chromatography-tandem mass spectrometry

建立了大豆提取物中16种多环芳烃(PAHs)和16种邻苯二甲酸酯类(PAEs)残留的快速检测方法。样品用水溶解、正己烷超声提取,提取液经乙二胺-N-丙基硅烷粉末分散固相萃取净化后,采用气相色谱-三重四极杆串联质谱法在选择反应监测模式下进行测定。结果表明:32种化合物在0.01～5.0μg/mL范围内呈良好线性,相关系数不低于0.99,方法的检测限为0.1～10.0μg/kg。在30～100μg/kg加标水平下的回收率为62.1%～126.9%,RSD为3.2%～15%。方法适用于大豆提取物中PAHs和PAEs的测定。

A rapid analytical method based on GC-MS/MS for the analysis of 16 polycyclic aromatic hydrocarbons （PAHs） and 16 phthalate esters （PAEs） residues in soybean extract has been developed. The sample was dissolved with water, extracted with n-hexane, cleaned-up by primary secondary amine （PSA）, using GC-MS/MS method in selected reaction monitoring mode （SRM） for determination. The results showed that the calibration curves of 32 compounds were linear in the range of 0. 0i ~ 5.0 μg/mL with correlation coefficients of no less than 0. 99 and the limits of detection （ LOD ） ranged from 0. 1 to 10. 0 μg/kg. The average spiked recoveries were in the range of 62. 1% - 126.9% at spiked levels of 30 - 100μg/kg with relative standard deviations（RSDs） of 3.2% - 15%. The method is suitable for the determination of 16 PAHs and 16 PAEs residues in soybean extract with advantages of easy operation, high accuracy and precision and simple operation.