气相色谱质谱法测定食用油中邻苯二甲酸酯

Determination of phthalate acid esters in edible oil by using gas chromatography-mass spectrometry

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 understand the current status of phthalic acid esters in edble oil in Anyang city. Methods Acetonitrile and methylence chloride 1 ： 2 （ V ： V ） was used as extractant,Florisil and PSA was used as purifying filler to the sample after extracting,the external standard method was adopted for quantifying in the GC-MS. Results A total of 16 phthalic acid esters were separated completely within 24 minutes,The calibration curves of 16 phthalic acid esters were linear（correlation coefficient r^2 〉0.99）within the range of 5μg/L-5 000μg/L. The recoveries were 80 %-105 %. The relative standard deviations（RSD） of the method was 〈10% ,and the limit of determination（LOD） was 0.12 μg/L-0.55μg/ L. Conclusion This method,by optimizing gas chromatographic conditions,makes 16 phthalic acid esters get better separation. The method is simple,accurate and sensitive,which is suitable for detection and confirmation of phthalic acid esters in edible oil.