油煎猪肉饼中6种氨基咔啉类杂环胺的检测方法及加工条件对其生成的影响

Determination of Six Amino-caroline Heterocyclic Aromatic Amines in Pan-fried Pork Patties and Effects of Processing Conditions on Their Formation

建立一种同时测定油煎猪肉饼中6种氨基咔啉类杂环胺(2-氨基-3-甲基-9H-吡啶并[2,3-b]吲哚、2-氨基-9H-吡啶并[2,3-b]吲哚、1-甲基-9H-吡啶并[3,4-b]吲哚、9H-吡啶并[3,4-b]吲哚、3-氨基-1,4-二甲基-5H-吡啶并[4,3-b]-吲哚和3-氨基-1-甲基-5H-吡啶并[4,3-b]吲哚)的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱检测方法,并研究加工条件对猪肉饼中6种氨基咔啉类杂环胺生成的影响。结果表明,待测杂环胺的最优提取和净化条件为:1 g样品中添加1.5 g NaCl、10 mL 1 mol/L NaOH溶液-乙腈(4∶6,V/V)提取,StrataTM-X-C柱净化,4 mL甲醇-氨水(90∶10,V/V)洗脱。6种杂环胺在相应质量浓度范围内线性良好,相关系数均大于0.996,方法检出限和方法定量限分别为0.02~0.15μg/kg和0.05~0.5μg/kg,回收率为64%~91%。油煎5 min后生成的6种杂环胺含量为9.50μg/kg。选用菜籽油、复合涂层锅、猪肉饼直径4 cm加工条件下,6种杂环胺生成量最高,分别为47.62、76.83μg/kg和29.33μg/kg。

A high performance liquid chromatography coupled to quadrupole-orbitrap high-resolution mass spectrometry method was developed for the simultaneous determination of six amino-carboline heterocyclic aromatic amines(HAAs)in pan-fried pork patties.The effects of processing conditions on the formation of these HAAs were also investigated.Results showed that the optimum extraction and purification conditions were as follows:1.0 g of the sample was extracted with 10 mL of 1 mol/L NaOH solution-acetonitrile(4:6,V/V)added with 1.5 g of NaCl,purified on a StrataTM-X-C column and eluted with methanol-ammonium hydroxide(90:10,V/V).The calibration curves for the six HAAs were linear in their respective concentration ranges with correlation coefficients greater than 0.996.The detection limit and quantification limit of the developed method were 0.02–0.15μg/kg and 0.05–0.5μg/kg,respectively.The recoveries of these HAAs were in the range of 64%–91%.The content of these six HAAs in pork patty pan-fried for 5 min was 9.50μg/kg.Pan-fried pork patties cooked with rapeseed oil,composite-coating pot,and patty thickness of 4 cm had the highest contents of HAAs,which were 47.62,76.83 and 29.33μg/kg,respectively.