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
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摘要: 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0.05-0.8 μg·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0.08-2.26 μg·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.Abstract: 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.
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Key words:
- phthalate esters /
- migration amount /
- blenders /
- GC-MS/MS
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