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| 食用油中两种塑化剂DBP和DEHP的气相色谱-质谱联用法测定及其风险暴露评估 |
| Determination of two plasticizers DBP and DEHP in edible oil by GC-MS and its risk exposure assessment |
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| DOI： |
| 中文关键词: DBP DEHP 气相色谱-质谱联用法 食用油 塑化剂 蒙特卡洛方法 风险评估 |
| 英文关键词:DBP DEHP gas chromatography-mass spectrometry(GC-MS) edible oil plasticizer Monte Carlo risk assessment |
| 基金项目:国家重点研发计划子课题（2018YFC1603405-02）；浙江省自然科学基金基础公益研究计划项目（LGN18C140002） |
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| 中文摘要: |
| 建立气相色谱-质谱联用法同时测定食用油中DBP和DEHP两种塑化剂的方法，并对114批次食用油样品进行检测，利用基于蒙特卡洛（Monte Carlo）统计模拟方法的水晶球（Crystal Ball）软件对检测结果进行风险评估，计算不同百分位数下DBP和DEHP的日均暴露量和风险指数。结果表明：样品经乙腈提取后，于40 ℃下氮吹至干，加入2.0 mL正己烷复溶，以40 mg十八烷基键合硅胶和60 mg N-丙基乙二胺净化后上机分析，采用Agilent HP-5MS毛细管色谱柱(30 m×0.25 mm，0.25 μm)进行分离，质谱选择电子轰击离子源（EI）和单离子检测扫描（SIM）模式下检测，DBP和DEHP标准曲线分别在0.084 6～1.353 6 μg/mL和0.120 9~1.934 4 μg/mL范围内呈现良好的线性关系，相关系数均大于0.99，检出限分别为0.06、0.08 mg/kg，3个质量浓度水平加标回收率在88.3%～111.2%之间，精密度在2.7%～5.6%之间；114批次食用油样品中9批次样品的塑化剂含量超风险值，两种塑化剂均有不同程度的风险，其中DBP的风险指数高于DEHP，且对7~10岁儿童的风险最高，需采取相应的应对措施，另外食用油中塑化剂含量对风险指数的影响最大。 |
| 英文摘要: |
| A method for the simultaneous determination of two plasticizers DBP and DEHP in edible oil by GC-MS was established. 114 batches of edible oil samples were detected, and the Crystal Ball software based on Monte Carlo statistical simulation method was used to evaluate the risk of the test results, and calculate the daily average exposure and risk index of DBP and DEHP under different percentiles. The resutls showed that the sample was extracted by acetonitrile, then the extract was dried with nitrogen at 40 ℃, redissolved by 2.0 mL n-hexane, and purified with 40 mg C18 and 60 mg PSA, then determined by GC-MS under the conditions of Agilent HP-5MS (30 m×0.25 mm，0.25 μm), electron impact ion source (EI) and single ion monitoring (SIM) mode. The calibration curves of DBP and DEHP showed good linearity in the range of 0.084 6-1.353 6 μg/mL and 0.120 9-1.934 4 μg/mL respectively, and the linear correlation coefficient was above 0.99. The detection limits were 0.06 mg/kg and 0.08 mg/kg respectively. The average recoveries of three mass concentrations ranged from 88.3% to 111.2%, and the precision were between 2.7% and 5.6%. Among the 114 batches of edible oil samples, the plasticizer content of 9 batches of samples exceeded the risk value, and the two plasticizers had different levels of risk. DBP had a higher risk index than DEHP, and the risk of DBP to children aged 7-10 was the highest, so corresponding measures should be taken. In addition, the plasticizers content in edible oil had the greatest impact on the risk index. |
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