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目的优化气相色谱和质谱条件,建立一种同时测定食用油中16种邻苯二甲酸酯的气相色谱质谱(GC-MS)方法。了解安阳市内销售的食用油中邻苯二甲酸酯含量现状。方法以乙腈和二氯甲烷1∶2(V∶V)的混合溶液作为萃取剂,用Florisil和PSA填料净化待提取的样品,采用外标法进行定量。结果 16种邻苯二甲酸酯在24min内流出并完全分离,在5~5 000μg/L范围内相关系数r均在0.99以上,样品加标回收率在80%~105%之间,相对标准偏差均小于10%,定性检出限为0.12~0.55μg/L。结论该方法通过优化气相色谱条件,使16种邻苯二甲酸酯得到较好分离。该方法操作简单、准确度和精密度高,适用于食用油中邻苯二甲酸酯的检测和确证。
Objective To optimize gas chromatography and mass spectrometry conditions and establish a simultaneous gas chromatography-mass spectrometry (GC-MS) method for simultaneous determination of 16 phthalates in edible oil. Learn Anyang city sales of edible oil in the phthalate content of the status quo. Methods A mixed solution of acetonitrile and dichloromethane (V: V) was used as extractant. Florisil and PSA fillers were used to purify the samples to be extracted and quantified by external standard method. Results 16 kinds of phthalate esters were eluted in 24 min and completely separated. The correlation coefficients r were all above 0.99 in the range of 5 ~ 5000 μg / L, and the spiked recoveries were between 80% and 105%. The relative standard Deviations were less than 10%, qualitative detection limit was 0.12 ~ 0.55μg / L. Conclusion This method can optimize the gas chromatographic conditions to get 16 kinds of phthalates well separated. The method has the advantages of simple operation, high accuracy and precision, and is suitable for the detection and confirmation of phthalates in cooking oil.