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    气相色谱-串联质谱法测定家用豆浆机中18种多环芳烃迁移量

    GC-MS/MS Determination of Migrated Amounts of 18 PAHs in Household Soybean Milk Machines

    • 摘要: 提出了家用豆浆机中18种多环芳烃(PAHs)迁移量的气相色谱-串联质谱法。取食品模拟液1 L在豆浆机正常运行下迁移60 min,迁移溶液经活化的C18固相萃取柱净化,用正己烷5 mL以3 mL·min-1的速率洗脱。净化液经无水硫酸钠干燥后,采用Agilent DB-17MS色谱柱进行气相色谱分离。质谱分析中采用电子轰击离子源和多反应监测模式。18种多环芳烃的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)在0.3~2.0 ng·L-1之间。按标准加入法在3个浓度水平上进行回收试验,回收率在78.5%~121%之间,测定值的相对标准偏差(n=6)在2.9%~12%之间。

       

      Abstract: A method was proposed for determination of migrated amounts of 18 PAHs in household soybean milk machines by GC-MS/MS. 1 L of food simulation was added in soybean milk machine and migrated for 60 min under the normal operation. The migrated solution was purified on activated C18 solid phase extraction (SPE) column and the analytes were eluted from the column with 5 mL of n-hexane (a flow rate of 3 mL·min-1). After dying with anhydrous sodium sulfate, the purified solution was separated by GC using Agilent DB-17MS column. EI and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 18 PAHs were found in definite ranges, with detection limits (3S/N) in the range of 0.3-2.0 ng·L-1. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 78.5%-121%, with RSDs (n=6) ranged from 2.9% to 12%.

       

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