气相色谱-串联质谱法测定家用搅拌机中21种邻苯二甲酸酯迁移量

Determination of the migration of the 21 phthalate esters in food blenders by GC-MS/MS

本文基于固相萃取-气相色谱串联质谱,建立了家用搅拌机中21种邻苯二甲酸酯(PAEs)迁移量的测定方法.基于搅拌机在运行过程中与食品接触特性,参照相关迁移实验标准,采用0.8 L 10%乙醇水溶液和4%乙酸水溶液两种模拟液在搅拌机正常工作下迁移30 min,以Oasis-HLB玻璃固相萃取柱对迁移溶液中待测物进行萃取浓缩,气相色谱-串联质谱检测,外标法定量.方法对于不同物质的定量限(LOQ)在0.05—0.8μg·L^(-1)之间,具有较高的灵敏度.在10%乙醇和4%乙酸两种模拟液中,低、中、高3个添加水平的平均回收率分别在78.5%—115.3%和78.8%—116.8%之间,相对标准偏差(RSD)分别在3.6%—12.5%和3.9%—11.2%之间.邻苯二甲酸酯在9款搅拌机实际样品中具有不同程度检出,迁移量0.08—2.26μg·L^(-1).该方法准确、灵敏,适用于家用搅拌机中邻苯二甲酸酯的迁移量检测.

A method was developed for the determination of the migration of 21 phthalate esters in food blenders using solid phase extraction （ SPE ） with gas chromatography-tandem mass spectrometry （GC-MS / MS）. Based on the contact characteristics of blenders during food processing, 0.8 L of food simulants were selected referring to relevant standards of migration experiment. Migration time was 30 min under the normal operation, then a HLB glass SPE column was used for extraction and enrichment of the analytes. The analytes were determined by GC-MS / MS and quantified by external standard method. The limits of quanification （LOQ） ranged from 0.05 μg·L-1 to 0.8 μg·L-1 . The average recoveries of 21 phthalate esters at three spiked levels ranged from 78.5％ to 115. 3％ in 10％ ethanol simulation, and from 78. 8％ to 116. 8％ in 4％ acetic acid simulation. The corresponding RSDs were from 3.6％ to 12.5％ and from 3.9％ to 11.2％ （n = 6）, respectively. Finally, the method was applied to detect the phthalate esters in nine blenders, and the migration amount ranged from 0.08 μg·L-1 to 2.26 μg·L-1 . The method is accurate, sensitive and suitable for the analysis of 21 phthalate esters in food blenders.