建立了超高效液相色谱-三重四极杆质谱( UPLC-MS/MS)同时测定食品级聚苯乙烯( PS)和聚乙烯( PE)色母粒中33种初级芳香胺( PAAs)的检测方法。PS色母粒用二氯甲烷溶解,超声提取后加入甲醇沉淀,并将提取液过石墨化碳固相萃取柱净化;PE色母粒用二氯甲烷超声溶胀提取;将 PS 色母粒过柱液和 PE 色母粒提取液浓缩,浓缩液用甲醇-水(1:9,v/v)定容至2 mL,0.22μm膜过滤后上机检测。采用 BEH Phenyl色谱柱(100 mm ×2.1 mm,1.7μm),以0.07%(v/v)甲酸甲醇溶液-水(1:9,v/v)为流动相,梯度洗脱分离,UPLC-MS/MS 多反应监测( MRM)模式检测,同位素内标法定量。优化了色谱分离条件、质谱碎裂电压、碰撞能量等,并考察了提取时间、提取溶剂、浓缩方式等对回收率的影响。33种 PAAs的方法检出限为6~10μg/kg,定量限为20~30μg/kg,2种不同基质样品在20、100、200μg/kg等3个添加水平的平均回收率为61.3%~119.8%,相对标准偏差( RSD)为1.4%~14.8%。本方法操作简便、快速、准确、灵敏度高,能满足相关测定要求。
A comprehensive analytical method based on ultra-performance liquid chromatogra-phy coupled with triple quadrupole mass spectrometry( UPLC-MS/MS)has been developed for the simultaneous determination of 33 primary aromatic amines( PAAs)in polystyrene( PS)and polyethylene( PE)masterbatches for foods. The PS masterbatches were dissolved with dichlo-romethane,and methanol was added to precipitate after extraction by ultrasound extraction. Then the extract was purified by passing through a carbon graphite solid phase extraction col-umn. The PE masterbatches were swelled and extracted with dichloromethane by ultrasound. The purified PS solution and PE extract were concentrated,and diluted to 2 mL with methanol-water(1:9,v/v),and filtered through the membranes of 0. 22 μm before UPLC-MS/MS analy-sis. The analytes were separated on a BEH Phenyl column(100 mm×2. 1 mm,1. 7 μm),eluted by gradient with 0. 07%( v/v ) formic acid in methanol-water( 1 :9,v/v ). The PAAs were detected by UPLC-MS/MS under multiple reaction monitoring( MRM )mode and quantified by the internal standard method. The separation conditions,fragment voltages and collision ener-gies were optimized. The impacts of extraction times,extraction solvents and concentration methods on recoveries were studied. The limits of detection for the 33 primary aromatic amines were 6—10 μg/kg,and the limits of quantitation were 20—30 μg/kg. The mean recoveries of the two different masterbatch products at three spiked levels of 20,100,200 μg/kg were 61. 3%—119. 8%,and the relative standard deviations were 1. 4%—14. 8%. The experimental results indi-cated that the method is simple,rapid,sensitive,accurate,and can meet the related require-ments for determination.
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