论文部分内容阅读
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 establish a gas chromatograph / triple quadrupole mass spectrometry (GC-MS / MS) method for the simultaneous determination of 16 phthalates in edible oils by gas chromatography and mass spectrometry, and to understand the production and sales in Anyang Of edible oil in the status of phthalate residues. Methods The samples were extracted with acetonitrile and cleaned up by solid-phase extraction cartridges. The sample was concentrated by liquid nitrogen and determined by gas chromatography-mass spectrometry (GC-MS / MS) and external standard method. Results 16 kinds of phthalates were completely separated within 23 min. The correlation coefficients r2 were all above 0.99 in the range of 5 ng / ml to 5000 ng / ml, and the recoveries were between 71.60% and 109.3% The standard deviation was less than 10% and the qualitative detection limit was 0.01 ng / ml ~ 0.45 ng / ml. Conclusion This method can get 16 kinds of phthalates well separated by choosing the appropriate gas chromatographic conditions. By selecting the appropriate characteristic ions and the appropriate energy, the secondary ions of characteristic ions are obtained and detected by GC-MS / MS Secondary ions, reducing interference, to avoid the appearance of false positives. 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.