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    固相萃取-高效液相色谱-三重四极杆质谱法测定食品加工电器中3种酚类内分泌干扰物的迁移量

    Determination of Migration of Three Phenolic Endocrine Disruptors from Food Processing Appliances by Solid-Phase Extraction Combined with High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

    • 摘要: 对咖啡壶和茶饮机选择10%(体积分数,下同)乙醇溶液作为食品模拟液,对豆浆机选择20%乙醇溶液作为食品模拟液。结合实际使用条件,设定食品加工电器工作状态,进行迁移试验:食品模拟液500 mL,温度100℃,迁移时间1 h。将迁移试验完毕后的食品模拟液静置冷却至室温,溶液中的双酚A、4-n-辛基酚、4-n-壬基酚经Oasis HLB固相萃取柱富集后,采用甲醇进行洗脱。洗脱液中3种酚类化合物在Waters XBridge C18色谱柱(2.1 mm×150 mm,3.5 μm)上分离,以甲醇和0.1%(体积分数)氨水溶液为流动相进行梯度洗脱后,进行串联质谱多反应监测模式分析。3种酚类化合物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)为0.001 3~0.002 5 mg·dm-2。加标回收率为84.6%~107%,测定值的相对标准偏差(n=6)为3.0%~9.1%。

       

      Abstract: 10% (φ, the same below) ethanol solution was selected as the food simulant for the coffee maker and the tea maker, and 20% ethanol solution was selected as the food simulant for the soybean milk maker. According to the actual conditions of use, the working status of food processing appliances were set and migration test was carried out under the follow conditions:food simulant of 500 mL, temperature of 100℃, migration time of 1 h. After the migration test, the food simulant was allowed to stand and cool to room temperature, and then bisphenol A, 4-n-octylphenol and 4-n-nonylphenol in the solution were enriched using an Oasis HLB solid-phase extraction column and eluted with methanol. The three phenolic compounds in the eluent were separated on a Waters XBridge C18 chromatographic column (2.1 mm×150 mm, 3.5 μm), with methanol and 0.1% ammonia solution (φ) as mobile phases for gradient elution. Multiple reaction monitoring mode was used for MS/MS analysis. Linear relationships were found between peak areas and mass concentraitons of the three phenolic compounds in definite ranges, with detection limits (3S/N) in the range of 0.001 3-0.002 5 mg·dm-2. Values of recovery obtained by standard addition method ranged from 84.6% to 107% and RSDs (n=6) ranged from 3.0% to 9.1%.

       

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