摘要
目的选取合适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/三重四极杆质谱(GC-MS/MS)方法,了解安阳市内生产和销售的食用油中邻苯二甲酸酯残留现状。方法样品经乙腈提取,固相萃取小柱净化,样品液氮吹浓缩后,用气相色谱质谱法(GC-MS/MS)测定,外标法定量。结果 16种邻苯二甲酸酯在23 min内完全分离,在5 ng/ml^5000 ng/ml范围内相关系数r2均在0.99以上,加标回收率在71.60%~109.3%之间,相对标准偏差均小于10%,定性检出限为0.01 ng/ml^0.45 ng/ml。结论该方法通过选取合适的气相色谱条件,使16种邻苯二甲酸酯得到较好分离;选取合适的特征离子、合适的能量,得到特征离子的二级离子,用GC-MS/MS检测二级离子,减少了干扰,避免假阳性的出现。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 select appropriate gas chromatography-mass spectrometry conditions,and establish a method for simultaneous determination of 16 phthalic acid esters in cooking oil by using gas chromatography-tandem mass spectrometry（ GC-MS/MS）,so as to understand the current status of phthalate esters residues in production and sale of cooking oil in Anyang city. Methods The phthalic acid esters in samples were extracted by acetonitrile,purified with silica / PSA column,concentrated by liquid nitrogen and then determined by GC / MS / MS using external standard method for quantitative anallysis. Results The 16 phthalic acid esters were separated completely within 23 min. The calibration curves of 16 phthalic acid esters were linear within the range of 5 ng / ml - 5000 ng / ml（ r^2 〉0. 99）. The recoveries were 71. 60% - 109. 3%. The relative standard deviations（ RSD） of the method was less than 10%,and the limit of determination（ LOD） was 0. 01 ng / ml - 0. 45 ng / ml. Conclusion The 16 kinds of phthalic acid esters were separated well by choosing suitable gas chromatographic conditions. Application of secondary ion of characteristic ion in GC-MS / MS detection can reduce the interference,thus avoiding the false positive. The method is simple,accurate and sensitive. It is suitable for analysis of phthalic acid esters in cooking oil.
出处
《中国卫生检验杂志》
北大核心
2014年第7期942-945,共4页
Chinese Journal of Health Laboratory Technology
关键词
邻苯二甲酸酯
固相萃取
气相色谱/三重四极杆质谱
食用油
Phthalic acid esters
Solid phase extraction
Gas chromatography-tandem mass spectrometry（GC /MS /MS）
Cooking oils
