同位素稀释-气相色谱-质谱法同时测定食用油中16种邻苯二甲酸酯类化合物
目的 建立一种同位素稀释-气相色谱-质谱法(GC-MS)同时测定食用油中16种邻苯二甲酸酯类化合物含量的方法。方法 样品经正己烷溶解, 乙腈提取, 经固相萃取柱净化, 以GC-MS在选择离子监测模式(SIM)下测定, 并采用同位素内标法定量分析。结果 空白基质加标回收实验添加水平分别为500.0、1000.0、2500.0 μg/kg时, 大豆油中16种邻苯二甲酸酯的回收率在67.4%~110.5%之间, 相对标准偏差在0.3%~12.7%之间; 黄油中16种邻苯二甲酸酯的回收率在60.5%~108.3%之间, 相对标准偏差在0.6%~12.7%之间。该方法在50.0~1000.0 μg/kg浓度范围内线性关系良好, 相关系数大于0.999, 方法检出限为500.0 μg/kg。结论 该方法灵敏度、精密度和检出限均符合实际样品检测要求, 适用于食用油中PAEs化合物的同时检测。
Objective To establish a method for determination of 16 kinds of phthalate esters (PAEs) in edible oils by gas chromatography-mass spectrometry (GC-MS) with isotopic dilution method. Methods The samples were dissolved with n-hexane and extracted with acetonitrile, and then purified by solid-phase column. Using GC-MS with selected ion monitoring (SIM), quantitative analysis was performed based upon isotopic internal method. Results The spiked recoveries at levels of 500.0, 1000.0, 2500.0 μg/kg used soybean oil and butter samples as blank matrix were respectively in the range of 67.4%~110.5% and 60.5%~108.3%. The relative standard deviations (RSDs) were respectively in the range of 0.3%~12.7% and 0.6%~12.7%. The experimental results showed that 16 kinds of PAEs had good linear relations in the range of 50.0~1000.0 μg/kg, the correlation coefficients were better than 0.999, and the limits of detection (LODs) of 16 PAEs were 500.0 μg/kg. Conclusion The sensitivity, precision and LOD can meet the requirements for the determination of the practical samples. This method can be used for the simultaneous detection of PAEs in edible oil samples.
标题：同位素稀释-气相色谱-质谱法同时测定食用油中16种邻苯二甲酸酯类化合物
英文标题：Determination of 16 kinds of phthalate esters in edible oils by gas chromatography-mass spectrometry with isotopic internal standards
作者：
杜娟 国家食品质量安全监督检验中心
马娇 国家食品质量安全监督检验中心
赵文霞 国家食品质量安全监督检验中心
宋杰 国家食品质量安全监督检验中心
中文关键词:气相色谱-质谱法,邻苯二甲酸酯类,食用油,同位素稀释法,
英文关键词:gas chromatography-mass spectrometry,phthalate esters,edible oil,isotopic dilution method,
发表日期：2015-12-06
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